Potassium Hydroxide → S-methyl N-[N'-methyl-N'-(dimethylaminosulfenyl)-carbamoyloxy]thioacetimidate

HRID 1447117노트

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HRID 1447117 반응식
[OH-].[K+].[CH3:3][SH-:4][C:5](=[N:7][OH:8])[CH3:6].[CH3:9][N:10]([S:14][N:15]([CH3:17])[CH3:16])[C:11](F)=[O:12]>C1CC2OCCOCCOC3C(OCCOCCOC2CC1)CCCC3.C1C=CC=CC=1>[CH3:9][N:10]([S:14][N:15]([CH3:17])[CH3:16])[C:11]([O:8][N:7]=[C:5]([S:4][CH3:3])[CH3:6])=[O:12]

참가 물질

6

반응물 3

HCID 14797Potassium HydroxideHCID 12799216N-methyl-N-(dimethylaminosulfenyl)carbamoyl fluorideHCID 178504139HCID 178504139, 화합물

생성물 1

HCID 54514859S-methyl N-[N'-methyl-N'-(dimethylaminosulfenyl)-carbamoyloxy]thioacetimidate수율 77.4%

시약·촉매·용매 2

HCID 85955Dicyclohexano-18-crown-6촉매HCID 241Benzene용매

실험 절차

Powdered potassium hydroxide (3.3 g), 5.2 g of S-methyl-N-hydroxythioacetimidate, 0.1 g dicyclohexyl-18-crown-6, and 200 ml of benzene were stirred at room temperature for 0.5 hr. Then 8.0 g of N-methyl-N-(dimethylaminosulfenyl)carbamoyl fluoride was added slowly at 28° C. The reaction temperature was held at 28°-32° C. with external cooling. The mixture was stirred for 1 hr., and then was washed with water until neutral. After drying (MgSO4), the solution was concentrated in vacuo, and the residue was recrystallized from diisopropyl ether to give 9.0 g (76 percent yield) of S-methyl N-[N'-methyl-N'-(dimethylaminosulfenyl)carbamoyloxy]Thioacetimidate, m.p. 68°-70° C.

후처리

  1. customwas held at 28°-32° C. with external cooling
  2. wash, and then was washed with water until neutral
  3. dry with materialAfter drying (MgSO4)
  4. concentrationthe solution was concentrated in vacuo
  5. customthe residue was recrystallized from diisopropyl ether

출처 및 근거

ORD 기록
ord-8fffadb1e6ee4033ba0a4cdf1a1b0fd3
출처 데이터셋
uspto-grants-1982_02
특허 번호
US04315928

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