Hydrogen chloride-ethyl acetate → 4-(1,7-diazaspiro[4.5]dec-7-yl)-7H-pyrrolo[2,3-d]pyrimidine

HRID 1912445ノート

反応式

HRID 1912445 の反応式
C(OC([N:8]1[C:12]2([CH2:17][CH2:16][CH2:15][N:14]([C:18]3[C:19]4[CH:26]=[CH:25][NH:24][C:20]=4[N:21]=[CH:22][N:23]=3)[CH2:13]2)[CH2:11][CH2:10][CH2:9]1)=O)(C)(C)C.Cl.C(OCC)(=O)C.Cl.CO>C(Cl)(Cl)Cl>[NH:8]1[C:12]2([CH2:17][CH2:16][CH2:15][N:14]([C:18]3[C:19]4[CH:26]=[CH:25][NH:24][C:20]=4[N:21]=[CH:22][N:23]=3)[CH2:13]2)[CH2:11][CH2:10][CH2:9]1

参加物

5

反応物 3

HCID 21866389Hydrogen chloride-ethyl acetateHCID 21893726Hydrochloride methanolHCID 582933867-(7H-pyrrolo[2,3-d]pyrimidin-4-yl)-1,7-diazaspiro[4.5]decane-1-carboxylic acid tert-butyl ester

生成物 1

HCID 582932974-(1,7-diazaspiro[4.5]dec-7-yl)-7H-pyrrolo[2,3-d]pyrimidine収率 69.5%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

To a solution of 7-(7H-pyrrolo[2,3-d]pyrimidin-4-yl)-1,7-diazaspiro[4.5]decane-1-carboxylic acid tert-butyl ester (60 mg) in chloroform (1.0 ml) were added 4M hydrochloric acid-ethyl acetate (1.5 ml) and 2M hydrochloric acid-methanol (0.5 ml), and the mixture was stirred at room temperature for 2.5 hours. The reaction mixture was concentrated under reduced pressure, and then azeotroped with toluene. The residue was neutralized by the addition of 4M aqueous sodium hydroxide solution, and thereto was added saturated aqueous sodium chloride solution. The mixture was extracted with chloroform. The separated organic solvent was concentrated under reduced pressure to give the titled compound (30 mg).

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customazeotroped with toluene
  3. additionThe residue was neutralized by the addition of 4M aqueous sodium hydroxide solution
  4. additionwas added saturated aqueous sodium chloride solution
  5. extractionThe mixture was extracted with chloroform
  6. concentrationThe separated organic solvent was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-cf85616bd4cd4d88a61d5c30ad58fec8
出典データセット
uspto-grants-2013_12
特許番号
US08609647B2

反応ノート

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