4-Nitrobenzenesulfonyl chloride → HCID 22674107、化合物

HRID 1005699ノート

反応式

HRID 1005699 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

HCID 22674107HCID 22674107、化合物

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 57417360Sodium chloride; water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7dab1240429149e88b968120772f4c55
出典データセット
uspto-grants-2004_09
特許番号
US06787534B2

反応ノート

読み込み中…