Potassium Carbonate → 2-(diethoxythiophosphoryloxy)-5,6-dihydro-4H-cyclopentathiazole

HRID 1288535노트

반응식

HRID 1288535 반응식
[S:1]1[C:5]2[CH2:6][CH2:7][CH2:8][C:4]=2[NH:3][C:2]1=[O:9].C(=O)([O-])[O-].[K+].[K+].[P:16](Cl)([O:21][CH2:22][CH3:23])([O:18][CH2:19][CH3:20])=[S:17]>CC(C)=O>[CH2:19]([O:18][P:16]([O:9][C:2]1[S:1][C:5]2[CH2:6][CH2:7][CH2:8][C:4]=2[N:3]=1)([O:21][CH2:22][CH3:23])=[S:17])[CH3:20]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 17305O,O-diethyl phosphorochloridothioateHCID 432867903,4,5,6-Tetrahydro-2H-cyclopenta[d][1,3]thiazol-2-one

생성물 1

HCID 867341092-(diethoxythiophosphoryloxy)-5,6-dihydro-4H-cyclopentathiazole

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of 21 g of 2,3,5,6,-tetrahydro-4H-cyclopentathiazoline-2-one, 21 g of potassium carbonate and 300 ml of acetone was refluxed for 1 hour and after the addition of 28 g of O,O-diethyl chlorothiophosphate thereto, the mixture was refluxed for 1 hour. The mineral salts were filtered off and the filtrate was distilled to dryness under reduced pressure. The residue was chromatographed over silica gel and was eluted with an 8-2 cyclohexane-ethyl acetate to obtain 4g of 2-(diethoxythiophosphoryloxy)-5,6-dihydro-4H-cyclopentathiazole with a refractive index of nD28 = 1.5348.

후처리

  1. temperaturewas refluxed for 1 hour
  2. temperaturethe mixture was refluxed for 1 hour
  3. filtrationThe mineral salts were filtered off
  4. distillationthe filtrate was distilled to dryness under reduced pressure
  5. customThe residue was chromatographed over silica gel
  6. washwas eluted with an 8-2 cyclohexane-ethyl acetate

출처 및 근거

ORD 기록
ord-d9a4820b77694722b8b35eecc1f22f65
출처 데이터셋
uspto-grants-1976_10
특허 번호
US03988444

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