Dimethylformamide → Ammonium Hydroxide

HRID 2044195노트

반응식

HRID 2044195 반응식
[Cl:1][C:2]1[C:7](C(O)=[O:9])=[C:6]([F:11])[C:5]([CH3:12])=[CH:4][CH:3]=1.C(Cl)Cl.C(Cl)(=O)C(Cl)=O.C[N:23]([CH:25]=[O:26])C>>[OH-:9].[NH4+:23].[Cl:1][C:2]1[C:7]([C:25]([NH2:23])=[O:26])=[C:6]([F:11])[C:5]([CH3:12])=[CH:4][CH:3]=1

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 6344DichloromethaneHCID 65578Oxalyl chlorideHCID 27736696-Chloro-2-fluoro-3-methylbenzoic acid

생성물 2

HCID 14923Ammonium Hydroxide수율 36%HCID 27736646-Chloro-2-fluoro-3-methylbenzamide

실험 절차

To 6-chloro-2-fluoro-3-methylbenzoic acid (10 g, 53 mmol) is added CH2Cl2 (60 mL), DMF (0.5 mL) and oxalyl chloride (9.25 mL, 106 mmol). The reaction mixture is allowed to stir until it reaches homogeneity and is then concentrated in vacuo. The residue is poured onto a 50:50 mixture of ice: 36% ammonium hydroxide to yield 6-chloro-2-fluoro-3-methylbenzamide.

후처리

  1. concentrationis then concentrated in vacuo
  2. additionThe residue is poured onto a 50:50 mixture of ice

출처 및 근거

ORD 기록
ord-6dc6942cca3b4cc0b730150c345d5ce0
출처 데이터셋
uspto-grants-2013_11
특허 번호
US08586782B2

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