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Water → 2-[(5-Chloro-2-fluoro-phenyl)-hydrazono]-propionic acid ethyl ester

HRID 853063
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반응식

HRID 853063 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([F:10])=[C:6]([NH:8][NH2:9])[CH:7]=1.[C:11]([O:16][CH2:17][CH3:18])(=[O:15])[C:12]([CH3:14])=O.O>ClCCl>[CH2:17]([O:16][C:11](=[O:15])[C:12](=[N:9][NH:8][C:6]1[CH:7]=[C:2]([Cl:1])[CH:3]=[CH:4][C:5]=1[F:10])[CH3:14])[CH3:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 12041Ethyl pyruvateHCID 2773732(5-chloro-2-fluorophenyl)hydrazine

생성물 1

HCID 865847132-[(5-Chloro-2-fluoro-phenyl)-hydrazono]-propionic acid ethyl ester수율 63%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

(5-Chloro-2-fluoro-phenyl)-hydrazine (22.5 g, 140 mmol) was dissolved in dichloromethane (80 mL). Ethyl pyruvate (16.3 mL, 140 mmol) was added slowly to this solution at room temperature. The mixture was stirred for another1 h at room temperature, added to water and extraxcted with dichloromethane. Organic phases were pooled, washed subsequently with hydrochloric acid (1 N) and brine and dried with MgSO4. Solvents were removed in vacuo and the residue was triturated with n-hexane to yield the title product as beige solid (22.8 g, 62.9%), ISP-MS: m/e=259.1 (M+H+).

후처리

  1. washwashed subsequently with hydrochloric acid (1 N) and brine
  2. dry with materialdried with MgSO4
  3. customSolvents were removed in vacuo
  4. customthe residue was triturated with n-hexane

출처 및 근거

ORD 기록
ord-54d6c07da5d34cd88ddbc15d3d1b82c5
출처 데이터셋
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07253281B2

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