Potassium Carbonate → HCID 88832108、化合物

HRID 1288534ノート

反応式

HRID 1288534 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 88832108HCID 88832108、化合物収率 37.2%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-fd872235d4ed41acb3386fff2de90dfb
出典データセット
uspto-grants-1976_10
特許番号
US03988444

反応ノート

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