ChemicalBook CAS DataBase List 1,3,3-Trimethyl-2-methyleneindoline

1,3,3-Trimethyl-2-methyleneindoline synthesis

11synthesis methods

Product Name:1,3,3-Trimethyl-2-methyleneindoline
CAS Number:118-12-7
Molecular formula:C12H15N
Molecular Weight:173.25

1640-39-7
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616-38-6 Synthesis

616-38-6
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118-12-7
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$5.00/5g

Yield:118-12-7 97.8%

Reaction Conditions:

at 180 - 220; under 22502.3 - 37503.8 Torr;Inert atmosphere;Sealed tube;Autoclave;

Steps:

1
Add 1 mol of 2,3,3-trimethyl-3H-indole and 3 mol of dimethyl carbonate to a 1L autoclave, and seal the autoclave with nitrogen for gas replacement. Then turn on the stirring, the temperature is raised to 180-220 °C, the pressure is 3.0-5.0 MPa, and the reaction is 6-8 h to the end of the reaction. Cool down and reduce pressure. Separate and recover dimethyl carbonate and by-product methanol under normal pressure and 85°C. Distill at 3-5KPa(A) under absolute pressure and 80-90°C to obtain methylated products.1,3,3-Trimethyl-2-methyleneindoline. The reaction conversion rate is 98.5%, and the quantitative product yield is 97.8%.

References:

CN112321480, 2021, A Location in patent:Paragraph 0013

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