Trimethyl phosphite → Phosphinecarboxylic acid, dimethoxy-, 4-methylphenyl ester, oxide

HRID 485288

반응식

C[O:2][P:3]([O:6][CH3:7])[O:4][CH3:5].Cl[C:9]([O:11][C:12]1[CH:17]=[CH:16][C:15]([CH3:18])=[CH:14][CH:13]=1)=[O:10]>>[C:15]1([CH3:18])[CH:16]=[CH:17][C:12]([O:11][C:9]([P:3](=[O:2])([O:6][CH3:7])[O:4][CH3:5])=[O:10])=[CH:13][CH:14]=1

참가 물질

반응물 2

HCID 8472Trimethyl phosphite

HCID 70304p-Tolyl chloroformate

생성물 1

HCID 512116Phosphinecarboxylic acid, dimethoxy-, 4-methylphenyl ester, oxide수율 93%

실험 절차

From 10.3 g (85 mmole) of trimethylphosphite and 10.3 g (60 mmole) of p-tolyl chloroformate (prepared according to M. J. Zabik and R. D. Scheutz J. Org. Chem. 32 (1967) 300). (100°, 2 hours) yield 93%. B.p.0.2 131°, nD20 1.4972. Analysis for C10H13O5P. Found (calculated): C 49.37 (49.18). H 5.53 (5.36), P 11.71 (12.69). NMR (CDCl3)δ: 2.40 (CH3), 3.92 and 4.12 (CH3O), 6.97-7.37 (aromatic protons).

후처리

custom(100°, 2 hours) yield 93%
customB.p.0.2 131°

출처 및 근거

ORD 기록: ord-a5b71eb669654b8d9f6cf8edc9c6ffd3
출처 데이터셋: uspto-grants-1985_08
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US04536400

연결된 노트

불러오는 중…