Trifluoroacetic acid → (2S,4S)-methyl 4-(4-amino-5-((3,5-dimethoxyphenyl)ethynyl)-7H-pyrrolo[2,3-d]pyrimidin-7-yl)pyrrolidine-2-carboxylate

HRID 516172노트

반응식

HRID 516172 반응식
[NH2:1][C:2]1[C:3]2[C:10]([C:11]#[C:12][C:13]3[CH:18]=[C:17]([O:19][CH3:20])[CH:16]=[C:15]([O:21][CH3:22])[CH:14]=3)=[CH:9][N:8]([C@@H:23]3[CH2:27][N:26](C(OC(C)(C)C)=O)[C@H:25]([C:35]([O:37][CH3:38])=[O:36])[CH2:24]3)[C:4]=2[N:5]=[CH:6][N:7]=1.C(O)(C(F)(F)F)=O>C(Cl)Cl>[NH2:1][C:2]1[C:3]2[C:10]([C:11]#[C:12][C:13]3[CH:14]=[C:15]([O:21][CH3:22])[CH:16]=[C:17]([O:19][CH3:20])[CH:18]=3)=[CH:9][N:8]([C@@H:23]3[CH2:27][NH:26][C@H:25]([C:35]([O:37][CH3:38])=[O:36])[CH2:24]3)[C:4]=2[N:5]=[CH:6][N:7]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 89871046(2S,4S)-1-tert-butyl 2-methyl 4-(4-amino-5-((3,5-dimethoxyphenyl)ethynyl)-7H-pyrrolo[2,3-d]pyrimidin-7-yl)pyrrolidine-1,2-dicarboxylate

생성물 1

HCID 89870853(2S,4S)-methyl 4-(4-amino-5-((3,5-dimethoxyphenyl)ethynyl)-7H-pyrrolo[2,3-d]pyrimidin-7-yl)pyrrolidine-2-carboxylate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of (2S,4S)-1-tert-butyl 2-methyl 4-(4-amino-5-((3,5-dimethoxyphenyl)ethynyl)-7H-pyrrolo[2,3-d]pyrimidin-7-yl)pyrrolidine-1,2-dicarboxylate (24 mg) obtained in Step 6 above in methylene chloride (2.0 ml) and TFA (2.0 ml) was stirred at room temperature for 30 minutes. The solvent was distilled off under reduced pressure, and the resulting residue was purified by basic silica gel column chromatography (developing solvent: chloroform/methanol). The title compound was thus obtained as a light-yellow, amorphous substance (11.9 mg). Physical properties: m/z [M+H]+ 422.1

후처리

  1. distillationThe solvent was distilled off under reduced pressure
  2. customthe resulting residue was purified by basic silica gel column chromatography (developing solvent: chloroform/methanol)

출처 및 근거

ORD 기록
ord-d5476b40c1664d3db21bbc7620a1a277
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09108973B2

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