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Sodium Hydroxide → 2-Chloro-5-{[4-(5-chloro-isoquinolin-6-yloxy)-cyclohexylamino]-methyl}-benzenesulfonamide

HRID 2370733
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HRID 2370733 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][NH:9][C@H:10]2[CH2:15][CH2:14][C@@H:13]([O:16][C:17]3[C:18]([Cl:27])=[C:19]4[C:24](=[CH:25][CH:26]=3)[CH:23]=[N:22][CH:21]=[CH:20]4)[CH2:12][CH2:11]2)=[CH:4][C:3]=1[S:28]([N:31]=CN(C)C)(=[O:30])=[O:29].[OH-].[Na+]>C(O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][NH:9][CH:10]2[CH2:15][CH2:14][CH:13]([O:16][C:17]3[C:18]([Cl:27])=[C:19]4[C:24](=[CH:25][CH:26]=3)[CH:23]=[N:22][CH:21]=[CH:20]4)[CH2:12][CH2:11]2)=[CH:4][C:3]=1[S:28]([NH2:31])(=[O:30])=[O:29]
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참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 178484402HCID 178484402, 화합물

생성물 1

HCID 592685782-Chloro-5-{[4-(5-chloro-isoquinolin-6-yloxy)-cyclohexylamino]-methyl}-benzenesulfonamide수율 48.4%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
65 °C

실험 절차

53 mg 2-Chloro-5-{cis-[4-(5-chloro-isoquinolin-6-yloxy)-cyclohexylamino]-methyl}-N-dimethylaminomethylene-benzenesulfonamide (74) were dissolved in 5 ml ethanol. 2 ml 2N NaOH were added and the mixture was heated to 65° C. After 5 h, the solvent was removed i. vac., the residue was dissolved in H2O and neutralized by adding 1 N HCl. The precipitate was filtered and dried, to yield 23 mg of the title compound as hydrochloride. Rt=0.89 min (Method #1). Detected mass: 480.2/484.2 (M+H+).

후처리

  1. customthe solvent was removed i
  2. dissolution, the residue was dissolved in H2O
  3. additionby adding 1 N HCl
  4. filtrationThe precipitate was filtered
  5. customdried

출처 및 근거

ORD 기록
ord-842c5f9ebf834beb925b663031b05a08
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08710228B2

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