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Sodium Hydroxide → 1-(5-(4-morpholino-6-((4-N-methylsulfonylpiperazin-1-yl)methyl)furo[3,2-d]pyrimidin-2-yl)pyridin-2-yl)urea

HRID 881370
ノート
印刷プレビュー

反応式

HRID 881370 の反応式
[O:1]1[CH2:6][CH2:5][N:4]([C:7]2[C:8]3[O:22][C:21]([CH2:23][N:24]4[CH2:29][CH2:28][N:27]([S:30]([CH3:33])(=[O:32])=[O:31])[CH2:26][CH2:25]4)=[CH:20][C:9]=3[N:10]=[C:11]([C:13]3[CH:14]=[CH:15][C:16]([NH2:19])=[N:17][CH:18]=3)[N:12]=2)[CH2:3][CH2:2]1.ClS([N:38]=[C:39]=[O:40])(=O)=O.[OH-].[Na+]>C(#N)C>[O:1]1[CH2:2][CH2:3][N:4]([C:7]2[C:8]3[O:22][C:21]([CH2:23][N:24]4[CH2:25][CH2:26][N:27]([S:30]([CH3:33])(=[O:32])=[O:31])[CH2:28][CH2:29]4)=[CH:20][C:9]=3[N:10]=[C:11]([C:13]3[CH:14]=[CH:15][C:16]([NH:19][C:39]([NH2:38])=[O:40])=[N:17][CH:18]=3)[N:12]=2)[CH2:5][CH2:6]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 70918Chlorosulfonyl isocyanateHCID 582339465-(4-morpholino-6-((4-N-methylsulfonylpiperazin-1-yl)methyl)furo[3,2-d]pyrimidin-2-yl)pyridin-2-amine

生成物 1

HCID 582338761-(5-(4-morpholino-6-((4-N-methylsulfonylpiperazin-1-yl)methyl)furo[3,2-d]pyrimidin-2-yl)pyridin-2-yl)urea

試薬・触媒・溶媒 1

HCID 6342Acetonitrile
溶媒

反応条件

温度
80 °C

実験手順

To a solution of 236 (1.0 eq) in acetonitrile (0.1M) at r.t. was added chlorosulfonyl isocyanate (10 eq) dropwise. The reaction was stirred for 40 minutes, then concentrated. To the residue was added 2N HCl and mixture was heated to 80° C. for 20 minutes. Reaction mixture was allowed to cool down to room temperature, and was neutralized with NaOH 6M. Mixture was then concentrated. The crude product was purified by reverse phase HPLC to give 6 mg of 247. MS (Q1) 517 (M+

後処理

  1. concentrationconcentrated
  2. additionTo the residue was added 2N HCl and mixture
  3. customReaction mixture
  4. temperatureto cool down to room temperature
  5. concentrationMixture was then concentrated
  6. customThe crude product was purified by reverse phase HPLC

出典と根拠

ORDレコード
ord-e0411f8f94ac451ba8c1b4fa022a5f75
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08993563B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート