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

HRID 2189293ノート

反応式

HRID 2189293 の反応式
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]

参加物

4

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-cacf9f2c559a46caaff31ab1e396297b
出典データセット
uspto-grants-2012_12
特許番号
US08324225B2

反応ノート

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