4-Amino-5-chloro-2-methoxybenzoic acid → Methyl 4-amino-5-chloro-2-methoxybenzoate

HRID 407121

反応式

HRID 407121 の反応式
[NH2:1][C:2]1[C:10]([Cl:11])=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4]([O:12][CH3:13])[CH:3]=1.[CH3:14][Si](C=[N+]=[N-])(C)C>C1(C)C=CC=CC=1.CO>[NH2:1][C:2]1[C:10]([Cl:11])=[CH:9][C:5]([C:6]([O:8][CH3:14])=[O:7])=[C:4]([O:12][CH3:13])[CH:3]=1

参加物

5

反応物 2

HCID 816264-Amino-5-chloro-2-methoxybenzoic acidHCID 167693Trimethylsilyldiazomethane

生成物 1

HCID 700493Methyl 4-amino-5-chloro-2-methoxybenzoate

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 1140Toluene溶媒

実験手順

To a solution of 4-amino-5-chloro-2-methoxybenzoic acid (1.008 g, 5.0 mmol) in a mixture of toluene (9 mL) and methanol (1 mL) at 0° C. was added (trimethylsilyl)diazomethane (2.0 M in hexane, 3.0 mL, 6.0 mmol) dropwise. The reaction mixture was then warmed to room temperature and stirred for 16 h. Excess (trimethylsilyl)diazomethane was quenched by adding acetic acid until the bright yellow color of the reaction mixture disappeared. The mixture was then concentrated in vacuo to give the title compound as an off-white solid, which was used without further purification.

後処理

  1. customExcess (trimethylsilyl)diazomethane was quenched
  2. additionby adding acetic acid until the bright yellow color of the reaction mixture
  3. concentrationThe mixture was then concentrated in vacuo

出典と根拠

ORDレコード
ord-5bb34760073c43ca8f9742c14fb559ae
出典データセット
uspto-grants-2014_06
特許番号
US08754223B2

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