Phenothiazine → Methallyl phosphonic acid diisopropyl ester

HRID 328544

반응식

[P:1]([O:10][CH:11]([CH3:13])[CH3:12])([O:6][CH:7]([CH3:9])[CH3:8])[O:2]C(C)C.C1C2NC3C(=CC=CC=3)SC=2C=CC=1.P([O-])([O-])[O-].[CH2:32](Cl)[C:33](=[CH2:35])[CH3:34]>>[CH:11]([O:10][P:1]([CH2:34][C:33](=[CH2:32])[CH3:35])(=[O:2])[O:6][CH:7]([CH3:8])[CH3:9])([CH3:12])[CH3:13]

참가 물질

반응물 4

HCID 7108Phenothiazine

HCID 8304Triisopropyl phosphite

HCID 112413-Chloro-2-methyl-1-propene

HCID 107908Phosphite

생성물 1

HCID 13953151Methallyl phosphonic acid diisopropyl ester

실험 절차

208 parts of triisopropyl phosphite, 1.5 parts of phenothiazine and 3.4 parts of Ni(CO)4 (corresponding to 2 mol %, based on the phosphite) are heated to 120°-130° C in a nitrogen atmosphere. 99 parts (corresponding to a 10% excess) of methallyl chloride are added dropwise over a period of 5 hours. 68 parts of isopropyl chloride (Bp: 35°-36° C) are distilled off through a column. The product is fractionated in vacuo through a column. Boiling point: 58°-63° C/0.25 Torr; Yield: 155 parts (70.5% of the theoretical): nD20 : 1.4312 Purity according to GC: 97.3%

후처리

temperatureare heated to 120°-130° C in a nitrogen atmosphere
distillation68 parts of isopropyl chloride (Bp: 35°-36° C) are distilled off through a column

출처 및 근거

ORD 기록: ord-8a9b74cc0103416abf1784aa9c51e649
출처 데이터셋: uspto-grants-1977_04
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US04017564

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