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

HRID 1527472노트

반응식

HRID 1527472 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-c6f8844dda9e48489b2bb2b724897a53
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09085555B2

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