Trifluoroacetic acid → [7-(1-ethyl-propyl)-7H-pyrrolo[2,3-d]pyrimidin-2-yl]-(4-piperazin-1-yl-phenyl)-amine

HRID 2189293노트

반응식

HRID 2189293 반응식
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:19]=[CH:18][C:17]([NH:20][C:21]3[N:22]=[CH:23][C:24]4[CH:29]=[CH:28][N:27]([CH:30]([CH2:33][CH3:34])[CH2:31][CH3:32])[C:25]=4[N:26]=3)=[CH:16][CH:15]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O>ClCCl>[CH2:31]([CH:30]([N:27]1[C:25]2[N:26]=[C:21]([NH:20][C:17]3[CH:18]=[CH:19][C:14]([N:11]4[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]4)=[CH:15][CH:16]=3)[N:22]=[CH:23][C:24]=2[CH:29]=[CH:28]1)[CH2:33][CH3:34])[CH3:32]

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 690753604-{4-[7-(1-ethyl-propyl)-7H-pyrrolo[2,3-d]pyrimidin-2-ylamino]-phenyl}-piperazine-1-carboxylic acid tert-butyl ester

생성물 1

HCID 58016034[7-(1-ethyl-propyl)-7H-pyrrolo[2,3-d]pyrimidin-2-yl]-(4-piperazin-1-yl-phenyl)-amine수율 99.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 4-{4-[7-(1-ethyl-propyl)-7H-pyrrolo[2,3-d]pyrimidin-2-ylamino]-phenyl}-piperazine-1-carboxylic acid tert-butyl ester (167 mg, 0.36 mmol) in dichloromethane (3 mL) is added trifluoroacetic acid (1 mL). The reaction mixture is stirred for 1 h and concentrated in vacuo. The residue is diluted with dichloromethane, washed with NaHCO3 solution, dried over Na2SO4, and concentrated in vacuo. Purification by preparative HPLC afforded 130 mg of [7-(1-ethyl-propyl)-7H-pyrrolo[2,3-d]pyrimidin-2-yl]-(4-piperazin-1-yl-phenyl)-amine as a yellowish solid.

후처리

  1. concentrationconcentrated in vacuo
  2. additionThe residue is diluted with dichloromethane
  3. washwashed with NaHCO3 solution
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated in vacuo
  6. customPurification by preparative HPLC

출처 및 근거

ORD 기록
ord-cacf9f2c559a46caaff31ab1e396297b
출처 데이터셋
uspto-grants-2012_12
특허 번호
US08324225B2

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