Methanol → 3-Aminomethyl-5-chloro-4-fluoro-benzoic acid methyl ester

HRID 1527472ノート

反応式

HRID 1527472 の反応式
[CH3:1][O:2][C:3](=[O:21])[C:4]1[CH:9]=[C:8]([Cl:10])[C:7]([F:11])=[C:6]([CH2:12][NH:13]C(OC(C)(C)C)=O)[CH:5]=1.C(O)(C(F)(F)F)=O.CO>C(Cl)Cl>[CH3:1][O:2][C:3](=[O:21])[C:4]1[CH:9]=[C:8]([Cl:10])[C:7]([F:11])=[C:6]([CH2:12][NH2:13])[CH:5]=1

参加物

5

反応物 3

HCID 887MethanolHCID 6422Trifluoroacetic acidHCID 682835653-(tert-Butoxycarbonylamino-methyl)-5-chloro-4-fluoro-benzoic acid methyl ester

生成物 1

HCID 682839273-Aminomethyl-5-chloro-4-fluoro-benzoic acid methyl ester

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 3-(tert-butoxycarbonylamino-methyl)-5-chloro-4-fluoro-benzoic acid methyl ester (4.25 g, 13.4 mmol) in CH2Cl2 (70 mL) was added TFA (10.3 mL, 134 mmol), and stirring was continued at RT overnight. Methanol was then added to the reaction mixture, and volatiles were removed in vacuo. The residue was taken up in methanol and concentrated again under reduced pressure to afford the title compound as a beige solid. MS (LC/MS): 218.0 [M+H]+; tR (HPLC conditions c): 3.10 min. The material thus obtained was used in the next reaction step without further purification.

後処理

  1. customwere removed in vacuo
  2. concentrationconcentrated again under reduced pressure

出典と根拠

ORDレコード
ord-c6f8844dda9e48489b2bb2b724897a53
出典データセット
uspto-grants-2015_07
特許番号
US09085555B2

反応ノート

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