Potassium Carbonate → HCID 21502749, 화합물

HRID 1288531노트

반응식

HRID 1288531 반응식
[S:1]1[C:5]2[CH2:6][CH2:7][CH2:8][CH2:9][C:4]=2[NH:3][C:2]1=[O:10].C(=O)([O-])[O-].[K+].[K+].[P:17](Cl)([O:22][CH2:23][CH3:24])([O:19][CH2:20][CH3:21])=[S:18]>CC(C)=O>[CH2:20]([O:19][P:17]([O:10][C:2]1[S:1][C:5]2[CH2:6][CH2:7][CH2:8][CH2:9][C:4]=2[N:3]=1)([O:22][CH2:23][CH3:24])=[S:18])[CH3:21]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 17305O,O-diethyl phosphorochloridothioateHCID 217932654,5,6,7-Tetrahydro-1,3-benzothiazol-2(3H)-one

생성물 1

HCID 21502749HCID 21502749, 화합물수율 59.5%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of 6.2 g of 2,3,4,5,6,7-hexahydrobenzothiazoline-2-one, 8.4 g of potassium carbonate and 300 ml of acetone was refluxed for 1 hour and after the addition of 11.4 g of O,O-diethyl chlorothiophosphate thereto, the mixture was refluxed for another hour. The mixture was stirred at room temperature for 24 hours and was filtered to remove mineral salts. The filtrate was concentrated to dryness by distillation under reduced pressure and the residue was chromatographed over silica gel. Elution with an 8-2 cyclohexane-ethyl acetate mixture yielded 7.3 g of 2-(diethoxythiophosphoryloxy)-4,5,6,7-tetrahydrobenzothiazole having a refractive index of nD22 = 1.532.

후처리

  1. temperaturewas refluxed for 1 hour
  2. temperaturethe mixture was refluxed for another hour
  3. filtrationwas filtered
  4. customto remove mineral salts
  5. concentrationThe filtrate was concentrated to dryness by distillation under reduced pressure
  6. customthe residue was chromatographed over silica gel
  7. washElution with an 8-2 cyclohexane-ethyl acetate mixture

출처 및 근거

ORD 기록
ord-7987a441840e4d0399024061a7e68716
출처 데이터셋
uspto-grants-1976_10
특허 번호
US03988444

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