Potassium Carbonate → HCID 53875402, 화합물

HRID 1834184노트

반응식

HRID 1834184 반응식
[OH:1][C:2]1[N:6]=[C:5]([S:7][CH3:8])[S:4][N:3]=1.[P:9](Cl)([O:14][CH2:15][CH3:16])([O:11][CH2:12][CH3:13])=[S:10].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH2:12]([O:11][P:9]([O:1][C:2]1[N:6]=[C:5]([S:7][CH3:8])[S:4][N:3]=1)([O:14][CH2:15][CH3:16])=[S:10])[CH3:13]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 17305O,O-diethyl phosphorochloridothioateHCID 178503579HCID 178503579, 화합물

생성물 1

HCID 53875402HCID 53875402, 화합물

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of 7.6 g of the product of Step A, 9.5 g of diethyl chlorothiophosphate and 7 g of potassium carbonate in 50 ml of acetone was stirred overnight at room temperature and the mixture was then filtered. The filtrate was concentrated by evaporation under reduced pressure and was chromatographed over silica. Elution with a 9-1 benzene-ethylacetate mixture yielded 3-(diethoxythiophosphoryloxy)-5-methylthio-1,2,4-thiadiazole with a refractive index of nD20 = 1.5534 and Rf=0.4.

후처리

  1. filtrationthe mixture was then filtered
  2. concentrationThe filtrate was concentrated by evaporation under reduced pressure
  3. customwas chromatographed over silica
  4. washElution with a 9-1 benzene-ethylacetate mixture

출처 및 근거

ORD 기록
ord-3d1b5b0f65304718aa4d036c1b1ec36c
출처 데이터셋
uspto-grants-1978_01
특허 번호
US04069319

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