4-Nitrobenzenesulfonyl chloride → HCID 22674107, 화합물

HRID 1173142노트

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HRID 1173142 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 compound synthesized using 6-amino-1-methoxyisoquinoline (Production Example 43b) and 4-nitrobenzenesulfonyl chloride in the same manner as in Synthetic Example 1b was processed in the same manner as in Production Example 170b, to reduce the nitro group thereof. The resulting compound was dissolved in pyridine and methanesulfonyl chloride was added thereto under ice-cooling, followed by stirring for 4 hours as it was. Brine was added thereto, followed by extracting with ethyl acetate. The extract was washed with brine and dried over anhydrous magnesium sulfate. After evaporating the solvent, the residue was purified by silica gel column and the resulting crystals were recrystallized from ethanol, to give the title compound.

후처리

  1. customThe compound synthesized
  2. temperatureunder ice-cooling
  3. extractionby extracting with ethyl acetate
  4. washThe extract was washed with brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customAfter evaporating the solvent
  7. customthe residue was purified by silica gel column
  8. customthe resulting crystals were recrystallized from ethanol

출처 및 근거

ORD 기록
ord-6832803b492d4221b50f476ba5b30a29
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07834049B2

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