Potassium Carbonate → 5-oxo-2,2,4-trimethyl-3-thiazoline O-[N-(di-n-butylaminosulphenyl)-N-methylcarbamoyl]oxime

HRID 1981372노트

반응식

HRID 1981372 반응식
[N:1](=[C:3]1[S:7][C:6]([CH3:9])([CH3:8])[N:5]=[C:4]1[CH3:10])[OH:2].C(=O)([O-])[O-].[K+].[K+].[CH2:17]([N:21]([CH2:28][CH2:29][CH2:30][CH3:31])[S:22][N:23]([CH3:27])[C:24](F)=[O:25])[CH2:18][CH2:19][CH3:20]>C(#N)C>[CH2:17]([N:21]([CH2:28][CH2:29][CH2:30][CH3:31])[S:22][N:23]([CH3:27])[C:24]([O:2][N:1]=[C:3]1[S:7][C:6]([CH3:9])([CH3:8])[N:5]=[C:4]1[CH3:10])=[O:25])[CH2:18][CH2:19][CH3:20]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 12799219N-(di-n-butylaminosulfenyl)-N-fluorocarbonyl-N-methylamineHCID 1362290545-Oxo-2,2,4-trimethyl-3-thiazoline oxime

생성물 1

HCID 545025405-oxo-2,2,4-trimethyl-3-thiazoline O-[N-(di-n-butylaminosulphenyl)-N-methylcarbamoyl]oxime

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

3.0 g (0.019 mol) of 5-oxo-2,2,4-trimethyl-3-thiazoline oxime are suspended in 10 ml of absolute acetonitrile. To the suspension at 0° C. there are successively added 5.5 g of anhydrous potassium carbonate and, dropwise, a solution of 4.52 g of N-(di-n-butylaminosulphenyl)-N-methylcarbamoyl fluoride in 10 ml of absolute acetonitrile. The reaction mixture is allowed to stir well at room temperature for 20 hours. Subsequently, the precipitated potassium salt is filtered off, and the filtrate is evaporated. Chromatography of the crude oily product on silica gel with ethyl acetate/toluene (1:3) as the eluent yields 5-oxo-2,2,4-trimethyl-3-thiazoline O-[N-(di-n-butylaminosulphenyl)-N-methylcarbamoyl]oxime, nD20 1.5200.

후처리

  1. customat 0° C.
  2. filtrationSubsequently, the precipitated potassium salt is filtered off
  3. customthe filtrate is evaporated

출처 및 근거

ORD 기록
ord-bf1d9ff86c1045608c73b762138fb7ee
출처 데이터셋
uspto-grants-1985_04
특허 번호
US04514566

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