Trichloromethanesulfenyl chloride → HCID 18788458, 화합물

HRID 129812

반응식

HRID 129812 반응식
[Cl:1][C:2](Cl)(Cl)[S:3]Cl.[CH3:7][C:8]1[CH:16]=[C:15]([CH3:17])[CH:14]=[C:13]([CH3:18])[C:9]=1[C:10]([NH2:12])=[NH:11].[OH-].[Na+]>ClCCl.O>[Cl:1][C:2]1[S:3][N:12]=[C:10]([C:9]2[C:8]([CH3:7])=[CH:16][C:15]([CH3:17])=[CH:14][C:13]=2[CH3:18])[N:11]=1

참가 물질

6

반응물 3

HCID 11666Trichloromethanesulfenyl chlorideHCID 14798Sodium HydroxideHCID 18788461HCID 18788461, 화합물

생성물 1

HCID 18788458HCID 18788458, 화합물수율 99.1%

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

2.2 g of trichloromethanesulfenyl chloride are introduced into a solution of 2 g of 2,4,6-trimethyl benzamidine in 16 ml of dichloromethane under an inert atmosphere at about -20° C., followed by the slow addition of 2 g of NaOH dissolved in 3.2 ml of water at about -10° C. After I hour at about -5° C., the precipitate formed is isolated and the organic phase is separated and washed with 6 ml of water. After being dried over K2CO3, it is concentrated under reduced pressure to give 2.8 g of the desired product in the form of an oil, which may be used without purification.

후처리

  1. customAfter I hour at about -5° C., the precipitate formed
  2. customis isolated
  3. customthe organic phase is separated
  4. washwashed with 6 ml of water
  5. dry with materialAfter being dried over K2CO3, it
  6. concentrationis concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-80152b1af913426387206ec895462f2e
출처 데이터셋
uspto-grants-1995_11
특허 번호
US05470855

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