Potassium Carbonate → HCID 53875402、化合物

HRID 1834184ノート

反応式

HRID 1834184 の反応式
[OH:1][C:2]1[N:6]=[C:5]([S:7][CH3:8])[S:4][N:3]=1.[P:9](Cl)([O:14][CH2:15][CH3:16])([O:11][CH2:12][CH3:13])=[S:10].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH2:12]([O:11][P:9]([O:1][C:2]1[N:6]=[C:5]([S:7][CH3:8])[S:4][N:3]=1)([O:14][CH2:15][CH3:16])=[S:10])[CH3:13]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 17305O,O-diethyl phosphorochloridothioateHCID 178503579HCID 178503579、化合物

生成物 1

HCID 53875402HCID 53875402、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of 7.6 g of the product of Step A, 9.5 g of diethyl chlorothiophosphate and 7 g of potassium carbonate in 50 ml of acetone was stirred overnight at room temperature and the mixture was then filtered. The filtrate was concentrated by evaporation under reduced pressure and was chromatographed over silica. Elution with a 9-1 benzene-ethylacetate mixture yielded 3-(diethoxythiophosphoryloxy)-5-methylthio-1,2,4-thiadiazole with a refractive index of nD20 = 1.5534 and Rf=0.4.

後処理

  1. filtrationthe mixture was then filtered
  2. concentrationThe filtrate was concentrated by evaporation under reduced pressure
  3. customwas chromatographed over silica
  4. washElution with a 9-1 benzene-ethylacetate mixture

出典と根拠

ORDレコード
ord-3d1b5b0f65304718aa4d036c1b1ec36c
出典データセット
uspto-grants-1978_01
特許番号
US04069319

反応ノート

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