4-Nitrobenzenesulfonyl chloride → HCID 22674107, 화합물

HRID 1005699노트

반응식

HRID 1005699 반응식
[NH2:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[C:8]([O:12][CH3:13])=[N:7][CH:6]=[CH:5]2.[N+:14]([C:17]1[CH:22]=[CH:21][C:20]([S:23](Cl)(=[O:25])=[O:24])=[CH:19][CH:18]=1)([O-])=O.[CH3:27][S:28](Cl)(=[O:30])=[O:29]>N1C=CC=CC=1.[Cl-].[Na+].O>[CH3:27][S:28]([NH:14][C:17]1[CH:22]=[CH:21][C:20]([S:23]([NH:1][C:2]2[CH:3]=[C:4]3[C:9](=[CH:10][CH:11]=2)[C:8]([O:12][CH3:13])=[N:7][CH:6]=[CH:5]3)(=[O:25])=[O:24])=[CH:19][CH:18]=1)(=[O:30])=[O:29]

참가 물질

6

반응물 3

HCID 74044-Nitrobenzenesulfonyl chlorideHCID 31297Methanesulfonyl chlorideHCID 226740451-Methoxyisoquinolin-6-amine

생성물 1

HCID 22674107HCID 22674107, 화합물

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 57417360Sodium chloride; water용매

실험 절차

The nitro group of the compound synthesized in the same manner as in Example 1, except using 6-amino-1-methoxyisoquinoline (Preparation Example 43) and 4-nitrobenzenesulfonyl chloride was reduced in the same manner as in Preparation Example 170. The resulting compound was dissolved in pyridine, and under ice-cooling, methanesulfonyl chloride was added thereto, followed by stirring as it was for 4 hours. Brine was added thereto, followed by extracting with ethyl acetate, The extract was washed with brine, dried over anhydrous magnesium sulfate and the solvent was evaporated. Then, the residue was purified by silica gel column, and the resulting crystals were recrystallized from ethanol, to give the title compound.

후처리

  1. customThe nitro group of the compound synthesized in the same manner as in Example 1
  2. customwas reduced in the same manner as in Preparation Example 170
  3. temperatureunder ice-cooling
  4. extractionby extracting with ethyl acetate
  5. washThe extract was washed with brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customthe solvent was evaporated
  8. customThen, the residue was purified by silica gel column
  9. customthe resulting crystals were recrystallized from ethanol

출처 및 근거

ORD 기록
ord-7dab1240429149e88b968120772f4c55
출처 데이터셋
uspto-grants-2004_09
특허 번호
US06787534B2

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