Potassium Carbonate → HCID 21502749、化合物

HRID 1288531ノート

反応式

HRID 1288531 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 21502749HCID 21502749、化合物収率 59.5%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7987a441840e4d0399024061a7e68716
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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