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CAS No. : | 137730-67-7 | MDL No. : | MFCD01632538 |
Formula : | C13H16ClN | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | CNFMPMUITJAJKC-UHFFFAOYSA-N |
M.W : | 221.73 | Pubchem ID : | 22509344 |
Synonyms : |
|
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P280-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H332-H335 | Packing Group: | N/A |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
76% | Method B; Spiro [indene-1, 4'-piperidine] hydrochloride (128.0 g, 560 mmol) is dissolved in ethanol (1.5 L) under a nitrogen atmosphere at 30 C. Diisopropylethylamine (407.4 mL, 1.68 mol) is added dropwise at 30 C over a period of 10 minutes, and is stirred for 20 minutes. Methyl 5-(bromomethyl) thiophene-2-carboxylate (~50 % pure by LCMS) (300 g, 1.27 mol) is added at 30 C and stirred at 30 C for 10 minutes and the mixture is heated to 60 C for 1 h 45 min. The reaction is monitored by TLC showed the presence of starting material. The reaction is stirred for 13 hours at 30 C. The reaction mixture is concentrated and dissolved in DCM (10 L). HQ (1 N, 1.5 L) is added dropwise with constant stirring and a white solid precipitates and is collected. The material is dissolved in DCM (1 L), stirred for 10 minutes, filtered, and dried under vacuum (44 C) to give the title compound (150.0 g, 76%). ESI/MS m/z 340.1 (M+H)+. |
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