ChemicalBook CAS DataBase List METHYLENEBIS(PHOSPHONIC DICHLORIDE)

METHYLENEBIS(PHOSPHONIC DICHLORIDE) synthesis

6synthesis methods

Product Name:METHYLENEBIS(PHOSPHONIC DICHLORIDE)
CAS Number:1499-29-2
Molecular formula:CH2Cl4O2P2
Molecular Weight:249.78

Methylenebisphosphonic acid tetrakis(trimethylsilyl) ester

53044-26-1
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1499-29-2
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Yield:1499-29-2 74 %

Reaction Conditions:

Stage #1: methylenebisphosphonic acid tetrakis(trimethylsilyl) esterwith oxalyl dichloride in dichloromethane;N,N-dimethyl-formamide at 20;Large scale;
Stage #2: in tert-butyl methyl ether at 20;Large scale;

Steps:

1

S3. Take 6kg of compound 2 obtained in S2, add it to 24L of dichloromethane, and then add (COCl)2(8.19kg, 5.65L) and N,N-dimethylformamide DMF (28.3g, 29.8mL), mix it at 20 °C, stir the reaction for 12h, filter and concentrate under reduced pressure to obtain crude product;S4. The crude product was mixed with methyl tert-butyl ether MTBE, pulped at 20 °C, filtered and dried after grinding for 12H, and white solid compound 3, that is, the product methylene diphosphorus chloride (3.40kg), with a yield of 74%.

References:

CN115651015,2023,A Location in patent:Paragraph 0040; 0044-0045

1660-94-2 Synthesis