Dimethylformamide → Ammonium Hydroxide

HRID 1811534ノート

反応式

HRID 1811534 の反応式
[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

参加物

6

反応物 4

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

生成物 2

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

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-36a79107114642328e54f2ecccfbd40d
出典データセット
uspto-grants-2013_01
特許番号
US08362294B2

反応ノート

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