Methanesulfonic Acid → 9-bromo-2-(3-hydroxypropyloxy)-5-(3-pyridylmethyl)-4H-pyrido[3,2,1-jk]carbazole-4-one methanesulfonate

HRID 1531017ノート

反応式

HRID 1531017 の反応式
[Br:1][C:2]1[CH:14]=[CH:13][C:12]2[C:11]3[C:6]4=[C:7]([C:20](=[O:30])[C:21]([CH2:23][C:24]5[CH:25]=[N:26][CH:27]=[CH:28][CH:29]=5)=[CH:22][N:5]4[C:4]=2[CH:3]=1)[CH:8]=[C:9]([O:15][CH2:16][CH2:17][CH2:18][OH:19])[CH:10]=3.[CH3:31][S:32]([OH:35])(=[O:34])=[O:33]>CO>[CH3:31][S:32]([OH:35])(=[O:34])=[O:33].[Br:1][C:2]1[CH:14]=[CH:13][C:12]2[C:11]3[C:6]4=[C:7]([C:20](=[O:30])[C:21]([CH2:23][C:24]5[CH:25]=[N:26][CH:27]=[CH:28][CH:29]=5)=[CH:22][N:5]4[C:4]=2[CH:3]=1)[CH:8]=[C:9]([O:15][CH2:16][CH2:17][CH2:18][OH:19])[CH:10]=3

参加物

4

反応物 2

HCID 6395Methanesulfonic AcidHCID 98724899-bromo-2-(3-hydroxypropyloxy)-5-(3-pyridylmethyl)-4H-pyrido [3,2,1-jk]carbazole-4-one

生成物 1

HCID 98724889-bromo-2-(3-hydroxypropyloxy)-5-(3-pyridylmethyl)-4H-pyrido[3,2,1-jk]carbazole-4-one methanesulfonate収率 89.4%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

9-bromo-2-(3-hydroxypropyloxy)-5-(3-pyridylmethyl)-4H-pyrido[3,2,1-jk]carbazole-4-one (250 mg) obtained in Example 110 was suspended in methanol (200 ml) and to the suspension was added a solution of methanesulfonic acid (57 mg) in methanol (5 ml) at room temperature. The mixture was stirred for 30 minutes. The solvent was evaporated under reduced pressure, and the resulting crude crystals were washed with a small amount of methanol and ether in succession to obtain the title compound (270 mg, 89%).

後処理

  1. customThe solvent was evaporated under reduced pressure
  2. washthe resulting crude crystals were washed with a small amount of methanol and ether in succession

出典と根拠

ORDレコード
ord-c730adfd030c422d9768f55f02bf3a77
出典データセット
uspto-grants-2001_03
特許番号
US06197768B1

反応ノート

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