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Triethylamine → 2-Methyl-2-methylsulfonylpropionaldoxime N-chloroacetyl-N-methylcarbamate

HRID 653089
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반응식

HRID 653089 반응식
[Cl:1][CH2:2][C:3]([N:5]([CH3:9])[C:6](Cl)=[O:7])=[O:4].[CH3:10][C:11]([S:16]([CH3:19])(=[O:18])=[O:17])([CH3:15])[CH:12]=[N:13][OH:14].C(N(CC)CC)C>C1(C)C=CC=CC=1>[CH3:10][C:11]([S:16]([CH3:19])(=[O:18])=[O:17])([CH3:15])[CH:12]=[N:13][OH:14].[Cl:1][CH2:2][C:3]([N:5]([CH3:9])[C:6](=[O:14])[O-:7])=[O:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 5189322-Methyl-2-(methylsulfonyl)propionaldehyde oximeHCID 13424133N-chloroacetyl-N-methylcarbamoyl chloride

생성물 1

HCID 867406792-Methyl-2-methylsulfonylpropionaldoxime N-chloroacetyl-N-methylcarbamate수율 125.8%

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

To a solution of 5.0 g (0.029 m) of N-chloroacetyl-N-methylcarbamoyl chloride dissolved in 40 ml of toluene was added 4.74 g (0.029 m) of 2-methyl-2-methylsulfonylpropionaldoxime dissolved in 35 ml. of toluene followed by a slow addition of 2.9 g (0.029 m) of triethylamine. The reaction mixture was stirred at ambient temperatures over a period of 3 days. The solid product was filtered. The filter cake was washed with water and hexane and air dried to afford 5.7 g of a white solid with a melting point of 120°-121° C.

후처리

  1. dissolutiondissolved in 35 ml
  2. filtrationThe solid product was filtered
  3. washThe filter cake was washed with water and hexane and air
  4. customdried

출처 및 근거

ORD 기록
ord-fb0af05423ba4377b273d6a5256239db
출처 데이터셋
uspto-grants-1987_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04675340

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