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

HRID 1531017노트

반응식

HRID 1531017 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-c730adfd030c422d9768f55f02bf3a77
출처 데이터셋
uspto-grants-2001_03
특허 번호
US06197768B1

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