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Methyl chloroformate → Methyl (1,1-dimethylethyl)-(3,3,3-trichloro-2-hydroxypropyl)carbamate

HRID 127955
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인쇄 미리보기

반응식

HRID 127955 반응식
[CH3:1][C:2]([NH:5][CH2:6][CH:7]([OH:12])[C:8]([Cl:11])([Cl:10])[Cl:9])([CH3:4])[CH3:3].C(N(CC)CC)C.[CH3:20][O:21][C:22](Cl)=[O:23]>ClCCl>[CH3:4][C:2]([N:5]([CH2:6][CH:7]([OH:12])[C:8]([Cl:11])([Cl:10])[Cl:9])[C:22](=[O:23])[O:21][CH3:20])([CH3:1])[CH3:3]
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참가 물질

5

반응물 3

HCID 6586Methyl chloroformateHCID 8471TriethylamineHCID 234710203-(Tert-butylamino)-1,1,1-trichloropropan-2-ol

생성물 1

HCID 54278558Methyl (1,1-dimethylethyl)-(3,3,3-trichloro-2-hydroxypropyl)carbamate수율 83.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a stirred solution of 5 grams of 3-(1,1-dimethylethylamino)-1,1,1-trichloro-2-propanol and 2.15 grams of triethylamine in 50 grams of dichloromethane, cooled to -60° C., 2.01 grams of methylchloroformate was added dropwise during 5 minutes. After allowing the reaction mixture to warm to ambient temperature during 1 hour, the mixture was stirred for 3 hours. The reaction mixture was evaporated under a reduced pressure of 100 mm. Hg to 5.6 grams of an oil which was crystallized from 50 grams of hexane to yield 5.2 grams of white methyl (1,1-dimethylethyl)-(3,3,3-trichloro-2-hydroxypropyl)carbamate melting 100°-101° C.

후처리

  1. customThe reaction mixture was evaporated under a reduced pressure of 100 mm. Hg to 5.6 grams of an oil which
  2. customwas crystallized from 50 grams of hexane

출처 및 근거

ORD 기록
ord-29a047cf61934b129d817411fe33fe77
출처 데이터셋
uspto-grants-1981_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04258060

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