Potassium Carbonate → HCID 88832108, 화합물

HRID 1288534노트

반응식

HRID 1288534 반응식
[S:1]1[C:5]2[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][C:4]=2[NH:3][C:2]1=[O:11].C(=O)([O-])[O-].[K+].[K+].[P:18](Cl)([O:23][CH2:24][CH3:25])([O:20][CH2:21][CH3:22])=[S:19]>CC(C)=O>[CH2:21]([O:20][P:18]([O:11][C:2]1[S:1][C:5]2[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][C:4]=2[N:3]=1)([O:23][CH2:24][CH3:25])=[S:19])[CH3:22]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 17305O,O-diethyl phosphorochloridothioateHCID 432867223,4,5,6,7,8-Hexahydro-2H-cycloheptathiazol-2-one

생성물 1

HCID 88832108HCID 88832108, 화합물수율 37.2%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of 8.5 g of 2,3,5,6,7,8-hexahydro-4H-cycloheptathiazoline-2-one, 7 g of potassium carbonate and 200 ml of acetone was refluxed for 1 hour and after addition of 9.5 g of O,O-diethyl chlorothiophosphate thereto, the mixture was refluxed 24 hours. The mixture was filtered to remove mineral salts and the filtrate was distilled to dryness under reduced pressure. The residue was chromatographed over silica gel and elution with an 8-2 cyclohexane-ethyl acetate mixture gave 6 g of 2-(diethoxythiophosphoryloxy)-5,6,7,8-tetrahydro-4H-cycloheptathiazole with a refractive index of nD19 = 1.5246.

후처리

  1. temperaturewas refluxed for 1 hour
  2. temperaturethe mixture was refluxed 24 hours
  3. filtrationThe mixture was filtered
  4. customto remove mineral salts
  5. distillationthe filtrate was distilled to dryness under reduced pressure
  6. customThe residue was chromatographed over silica gel and elution with an 8-2 cyclohexane-ethyl acetate mixture

출처 및 근거

ORD 기록
ord-fd872235d4ed41acb3386fff2de90dfb
출처 데이터셋
uspto-grants-1976_10
특허 번호
US03988444

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