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Potassium Carbonate → 2-Cyano-3-(dimethoxythiophosphoryloxy)-5-phenylthiophene

HRID 263028
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인쇄 미리보기

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HRID 263028 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]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)=[CH:19][C:20]=1[OH:21])#[N:15]>CC(C)=O>[C:14]([C:16]1[S:17][C:18]([C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=2)=[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 21317938HCID 21317938, 화합물

생성물 1

HCID 541990462-Cyano-3-(dimethoxythiophosphoryloxy)-5-phenylthiophene수율 79%

시약·촉매·용매 1

HCID 180Acetone용매

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 10.5 g of 2-cyano-3-hydroxy-5-phenyl-thiophene in 120 ml of acetone and the mixture was stirred at 20° C. for 15 hours and was then filtered. The filtrate was evaporated to dryness and the crystal residue was empasted with petroleum ether. The crystals were then crystallized from isopropyl ether to obtain 12.8 g of 2-cyano-3-(dimethoxythiophosphoryloxy)-5-phenylthiophene melting at 95° C.

후처리

  1. filtrationwas then filtered
  2. customThe filtrate was evaporated to dryness
  3. customThe crystals were then crystallized from isopropyl ether

출처 및 근거

ORD 기록
ord-6fe98b1acfe84105b8a74768c904c7d5
출처 데이터셋
uspto-grants-1979_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04155996

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