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

HRID 65589
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인쇄 미리보기

반응식

HRID 65589 반응식
C(=O)([O-])[O-].[K+].[K+].[P:7](Cl)([O:11][CH3:12])([O:9][CH3:10])=[S:8].[C:14]([C:16]1[S:17][C:18]([O:22][CH2:23][CH2:24][CH2:25][CH3:26])=[CH:19][C:20]=1[OH:21])#[N:15]>C(#N)C>[C:14]([C:16]1[S:17][C:18]([O:22][CH2:23][CH2:24][CH2:25][CH3:26])=[CH:19][C:20]=1[O:21][P:7]([O:11][CH3:12])([O:9][CH3:10])=[S:8])#[N:15]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 17304Dimethyl phosphorochloridothionateHCID 213179005-Butoxy-3-hydroxythiophene-2-carbonitrile

생성물 1

HCID 545276212-Cyano-3-(dimethoxythiophosphoryloxy)-5-n-butoxy-thiophene수율 68.9%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
20 °C

실험 절차

7 g of potassium carbonate and 8 g of O,O-dimethyl 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 then filtered. The filtrate was evaporated to dryness and the residue was chromatographed over silica gel. Elution with benzene yielded 11 g of 2-cyano-3-(dimethoxythiophosphoryloxy)-5-n-butoxy-thiophene with a refractive index of nD20 = 1.5375.

후처리

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

출처 및 근거

ORD 기록
ord-d5f22fac622f4f12bc67103271588dd4
출처 데이터셋
uspto-grants-1978_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04128562

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