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

HRID 407121

반응식

HRID 407121 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 887Methanol용매HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5bb34760073c43ca8f9742c14fb559ae
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08754223B2

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