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N,N-Dimethylglycine → Rac-1-[3-(4-amino-3-iodo-1h-pyrazolo[3,4-d]pyrimidin-1-yl)tetrahydro-1h-1-pyrrolyl]-2-(dimethylamino)-1-ethanone

HRID 2056127
ノート
印刷プレビュー

反応式

HRID 2056127 の反応式
Cl.[I:2][C:3]1[C:11]2[C:6](=[N:7][CH:8]=[N:9][C:10]=2[NH2:12])[N:5]([CH:13]2[CH2:17][CH2:16][NH:15][CH2:14]2)[N:4]=1.[CH3:18][N:19]([CH3:24])[CH2:20][C:21](O)=[O:22].ON1C2N=CC=CC=2N=N1.Cl.CN(C)CCCN=C=NCC.C(N(C(C)C)CC)(C)C>ClCCl.O>[NH2:12][C:10]1[N:9]=[CH:8][N:7]=[C:6]2[N:5]([CH:13]3[CH2:17][CH2:16][N:15]([C:21](=[O:22])[CH2:20][N:19]([CH3:24])[CH3:18])[CH2:14]3)[N:4]=[C:3]([I:2])[C:11]=12
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 673N,N-DimethylglycineHCID 81531DiisopropylethylamineHCID 181649HOAtHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 223473313-iodo-1-tetrahydro-1H-3-pyrrolyl-1H-pyrazolo[3,4-d]pyrimidin-4-amine hydrochloride

生成物 1

HCID 69203801
Rac-1-[3-(4-amino-3-iodo-1h-pyrazolo[3,4-d]pyrimidin-1-yl)tetrahydro-1h-1-pyrrolyl]-2-(dimethylamino)-1-ethanone
収率 67%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of rac-3-iodo-1-tetrahydro-1H-3-pyrrolyl-1H-pyrazolo[3,4-d]pyrimidin-4-amine monohydrochloride (0.367 g, 1.00 mmol) in dichloromethane (10 mL) was added 2-(dimethylamino)acetic acid (0.134 g, 1.30 mmol), 1-hydroxy-7-azabenzotriazole (0.150 g, 1.10 mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (0.249 g, 1.30 mmol), and diisopropylethyl amine (0.65 g, 0.87 mL, 5.0 mmol). The reaction mixture stirred at room temperature for 18 h and was then poured into water (10 mL). The organic phase was separated and washed with brine (10 mL), dried over anhydrous magnesium sulfate, filtered, and concentrated to afford rac-1-[3-(4-amino-3-iodo-1H-pyrazolo[3,4-d]pyrimidin-1-yl)tetrahydro-1H-1-pyrrolyl]-2-(dimethylamino)-1-ethanone as a yellow-orange solid (0.278 g, 67%) which was used in subsequent reactions without further purification.

後処理

  1. customThe organic phase was separated
  2. washwashed with brine (10 mL)
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-ad1c666f2c564e739c79754513921ba5
出典データセット
uspto-grants-2008_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07332497B2

反応ノート

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