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Hydrogen Sulfide → HCID 20330468, 화합물

HRID 918569
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HRID 918569 반응식
[Na].[CH3:2][C:3]1[C:8]([O:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])=[C:7]([CH2:15][O:16][C:17]([O:19][CH2:20][CH3:21])=[O:18])[C:6]([CH2:22]Cl)=[CH:5][N:4]=1.[SH2:24]>CN(C)C=O>[CH3:2][C:3]1[C:8]([O:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])=[C:7]([CH2:15][O:16][C:17]([O:19][CH2:20][CH3:21])=[O:18])[C:6]([CH2:22][SH:24])=[CH:5][N:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 402Hydrogen Sulfide2회HCID 5360545SodiumHCID 203304722-Methyl-3-ethoxycarbonyloxy-4-ethoxycarbonyloxymethyl-5-chloromethylpyridine

생성물 1

HCID 20330468HCID 20330468, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 0.4 moles sodium in absolute dimethylformamide is saturated by passing in hydrogen sulfide for 5 hours. There is then added in portions 0.05 moles of 2-methyl-3-ethoxycarbonyloxy-4-ethoxycarbonyloxymethyl-5-chloromethylpyridine and the mixture stirred overnight at room temperature with hydrogen sulfide slowly bubbling through the mixture. The reaction mixture is then concentrated in vacuo and taken up between ethyl acetate and water containing acetic acid. The ethyl acetate layer is removed, dried over sodium sulfate and concentrated to give 2-methyl-3-ethoxycarbonyloxy-4-ethoxycarbonyloxymethyl-5-mercaptomethylpyridine.

후처리

  1. customslowly bubbling through the mixture
  2. concentrationThe reaction mixture is then concentrated in vacuo
  3. additioncontaining acetic acid
  4. customThe ethyl acetate layer is removed
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-94e1137edd204489aef9a1e7fad3111f
출처 데이터셋
uspto-grants-1976_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03971797

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