Potassium Carbonate → 2-Cyano-3-(diethoxythiophosphoryloxy)-5-n-butoxy-thiophene

HRID 263033

반응식

HRID 263033 반응식
C(=O)([O-])[O-].[K+].[K+].[P:7](Cl)([O:12][CH2:13][CH3:14])([O:9][CH2:10][CH3:11])=[S:8].[C:16]([C:18]1[S:19][C:20]([O:24][CH2:25][CH2:26][CH2:27][CH3:28])=[CH:21][C:22]=1[OH:23])#[N:17]>C(#N)C>[C:16]([C:18]1[S:19][C:20]([O:24][CH2:25][CH2:26][CH2:27][CH3:28])=[CH:21][C:22]=1[O:23][P:7]([O:12][CH2:13][CH3:14])([O:9][CH2:10][CH3:11])=[S:8])#[N:17]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 17305O,O-diethyl phosphorochloridothioateHCID 213179005-Butoxy-3-hydroxythiophene-2-carbonitrile

생성물 1

HCID 544164262-Cyano-3-(diethoxythiophosphoryloxy)-5-n-butoxy-thiophene수율 80.6%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
20 °C

실험 절차

7 g of potassium carbonate and 9.4 g of O,O-diethyl chlorothiophosphate were added to a solution of 9.8 g of 2-cyano-3-hydroxy-5-n-butoxy-thiophene in 150 ml of acetonitrile and the mixture was stirred for 24 hours at 20° C. and was filtered. The filtrate was evaporated to dryness under reduced pressure and the residue was chromatographed over silica gel. Elution with benzene yielded 14 g of 2-cyano-3-(diethoxythiophosphoryloxy)-5-n-butoxy-thiophene with a refractive index of nD20 =1.525.

후처리

  1. filtrationwas filtered
  2. customThe filtrate was evaporated to dryness under reduced pressure
  3. customthe residue was chromatographed over silica gel
  4. washElution with benzene

출처 및 근거

ORD 기록
ord-50c477b0f52c4dcbb3707af80acb45b0
출처 데이터셋
uspto-grants-1979_05
특허 번호
US04155996

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