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Potassium Carbonate → HCID 85518231, 화합물

HRID 1905793
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HRID 1905793 반응식
[C:1]([CH:3](C#N)[CH2:4][S:5][CH2:6][CH:7](C#N)[C:8]#[N:9])#[N:2].C(=O)([O-])[O-].[K+].[K+].[Br:20]Br>ClC(Cl)C>[C:1]([CH2:3][CH2:4][S:5][CH:6]=[C:7]([Br:20])[C:8]#[N:9])#[N:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium Carbonate2회HCID 24408BromineHCID 88229003HCID 88229003, 화합물

생성물 1

HCID 85518231HCID 85518231, 화합물수율 17.2%

시약·촉매·용매 1

HCID 63651,1-Dichloroethane용매

반응 조건

온도
40 °C

실험 절차

28 g of bis-cyanoethyl sulphide were dissolved in 50 ml of dichloroethane, and 110 g of potassium carbonate were added. 64 g of bromine were then added dropwise at 20° to 30° C. The mixture was stirred at 40° C. for 16 hours, a further 40 g of potassium carbonate were added and the mixture was stirred at 60° C. for 16 hours. The mixture was filtered, the filtrate was washed with water and concentrated and the residue was chromatographed. 5.5 g of 2-bromo-2-cyano-vinyl 2-cyano-ethyl sulphide were obtained as an oil, 1H-NMR: δ=2.6-3.0 (2H), 3.0-3.4 (2H) and 7.5-7.9 (1H).

후처리

  1. stirringthe mixture was stirred at 60° C. for 16 hours
  2. filtrationThe mixture was filtered
  3. washthe filtrate was washed with water
  4. concentrationconcentrated
  5. customthe residue was chromatographed

출처 및 근거

ORD 기록
ord-7b237a94b48f419780f04e85b50bc0d4
출처 데이터셋
uspto-grants-1987_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04647687

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