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Hydrazine → HCID 178497541, 화합물

HRID 1978194
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HRID 1978194 반응식
[CH3:1][O:2][C:3](=[O:17])[C:4]1[CH:9]=[CH:8][C:7]([CH2:10][CH:11]=[CH:12][N:13](C)C)=[CH:6][C:5]=1[Cl:16].[NH2:18]N>C(O)(=O)C>[CH3:1][O:2][C:3](=[O:17])[C:4]1[CH:9]=[CH:8][C:7]([C:10]2[CH:11]=[CH:12][NH:13][N:18]=2)=[CH:6][C:5]=1[Cl:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 9321HydrazineHCID 545013412-Chloro-4-(3-dimethylamino-2-propen-1-yl)-benzoic acid methyl ester

생성물 1

HCID 178497541HCID 178497541, 화합물수율 94.1%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A solution of 2-chloro-4-(3-dimethylamino-2-propen-1-yl)-benzoic acid methyl ester of Step B (6.13 g, 22.9 mmol) and anhydrous hydrazine (1.44 mL, 45.8 mmol) in 15 mL of glacial acetic acid was heated at 90° C. for 30 minutes. The reaction mixture was concentrated in vacuo and the residue partitioned between ethyl acetate and water. The organic layer was washed with water and brine and dried over sodium sulfate. The solvent was evaporated and the residual solid triturated with diethyl ether-hexane to give the title compound (5.1 g) as an orange solid.

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후처리

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. customthe residue partitioned between ethyl acetate and water
  3. washThe organic layer was washed with water and brine
  4. dry with materialdried over sodium sulfate
  5. customThe solvent was evaporated
  6. customthe residual solid triturated with diethyl ether-hexane

출처 및 근거

ORD 기록
ord-1fa6c5236a814e8faa386d789bf0bc95
출처 데이터셋
uspto-grants-2001_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06235900B1

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