Hydrochloric Acid → 1-({[2-(Benzylthio)-6-chloropyrimidin-4-yl]amino}sulfonyl)-N,N-dimethyl-D-prolinamide

HRID 424664ノート

反応式

HRID 424664 の反応式
[H-].[Na+].[NH2:3][S:4]([N:7]1[CH2:16][CH2:15][CH2:14][C@@H:8]1[C:9]([N:11]([CH3:13])[CH3:12])=[O:10])(=[O:6])=[O:5].[CH2:17]([S:24][C:25]1[N:30]=[C:29](NS(C)(=O)=O)[CH:28]=[C:27](NCCO)[N:26]=1)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.[ClH:40]>CN(C=O)C>[CH2:17]([S:24][C:25]1[N:30]=[C:29]([NH:3][S:4]([N:7]2[CH2:16][CH2:15][CH2:14][C@@H:8]2[C:9]([N:11]([CH3:13])[CH3:12])=[O:10])(=[O:6])=[O:5])[CH:28]=[C:27]([Cl:40])[N:26]=1)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 24758Sodium hydrideHCID 57833129N-{2-(Benzylthio)-6-[(2-hydroxyethyl)amino]pyrimidin-4-yl}methanesulfonamideHCID 667020511-(Aminosulfonyl)-N,N-dimethyl-D-prolinamide

生成物 1

HCID 866398311-({[2-(Benzylthio)-6-chloropyrimidin-4-yl]amino}sulfonyl)-N,N-dimethyl-D-prolinamide

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

60% Sodium hydride (0.42 g) was added to a solution of the subtitle product of step iii) (1.50 g) in DMF (20 ml) at 0° C. This mixture was stirred for 1 h and then a solution of the subtitle product of Example 19 step (1.60 g) in DMF (5 ml) was added dropwise. The mixture was allowed to reach room temperature and stirred there for 2 days. To the mixture was added aqueous hydrochloric acid (100 ml) and the resulting precipitate was filtered. This solid was then stirred with EtOAc (200 ml) and filtered to afford the subtitle compound as a solid. Yield: 2.0 g.

後処理

  1. customto reach room temperature
  2. stirringstirred there for 2 days
  3. filtrationthe resulting precipitate was filtered
  4. stirringThis solid was then stirred with EtOAc (200 ml)
  5. filtrationfiltered

出典と根拠

ORDレコード
ord-d4a4f5c0daca464e8cd7645920ff4bbf
出典データセット
uspto-grants-2012_01
特許番号
US08106063B2

反応ノート

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