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

HRID 424664노트

반응식

HRID 424664 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d4a4f5c0daca464e8cd7645920ff4bbf
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08106063B2

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