tert-Butyl methyl ether → 1-(1-[2-(7-methoxy-2,2-dimethyl-4-oxochroman-8-yl)ethyl]piperidin-4-yl}-N-methyl-1H-indole-6-carboxamide maleate

HRID 495011ノート

反応式

HRID 495011 の反応式
[CH3:1][O:2][C:3]1[C:12]([CH2:13][CH2:14][N:15]2[CH2:20][CH2:19][CH:18]([N:21]3[C:29]4[C:24](=[CH:25][CH:26]=[C:27]([C:30]([NH:32][CH3:33])=[O:31])[CH:28]=4)[CH:23]=[CH:22]3)[CH2:17][CH2:16]2)=[C:11]2[C:6]([C:7](=[O:36])[CH2:8][C:9]([CH3:35])([CH3:34])[O:10]2)=[CH:5][CH:4]=1.[C:37]([OH:44])(=[O:43])/[CH:38]=[CH:39]\[C:40]([OH:42])=[O:41].COC(C)(C)C>O1CCCC1>[C:37]([OH:44])(=[O:43])/[CH:38]=[CH:39]\[C:40]([OH:42])=[O:41].[CH3:1][O:2][C:3]1[C:12]([CH2:13][CH2:14][N:15]2[CH2:20][CH2:19][CH:18]([N:21]3[C:29]4[C:24](=[CH:25][CH:26]=[C:27]([C:30]([NH:32][CH3:33])=[O:31])[CH:28]=4)[CH:23]=[CH:22]3)[CH2:17][CH2:16]2)=[C:11]2[C:6]([C:7](=[O:36])[CH2:8][C:9]([CH3:34])([CH3:35])[O:10]2)=[CH:5][CH:4]=1

参加物

5

反応物 3

HCID 15413tert-Butyl methyl etherHCID 444266Maleic AcidHCID 11677552E-2110 free base

生成物 1

HCID 688561021-(1-[2-(7-methoxy-2,2-dimethyl-4-oxochroman-8-yl)ethyl]piperidin-4-yl}-N-methyl-1H-indole-6-carboxamide maleate収率 90.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

1-{1-[2-(7-Methoxy-2,2-dimethyl-4-oxochroman-8-yl)ethyl]piperidin-4-yl}-N-methyl-1H-indole-6-carboxamide (105 mg) was dissolved in tetrahydrofuran (10 ml). Thereafter, a tetrahydrofuran solution (10 ml) containing maleic acid (25 mg) was added to the reaction solution at room temperature. Thereafter, t-butyl methyl ether was added thereto at room temperature, and the obtained mixture was then concentrated under a reduced pressure. Diethyl ether was added to the residue for solidification. This suspension was stirred for 10 minutes while cooling on ice, and a solid was then collected by filtration. The solid was washed with diethyl ether, so as to obtain the subject compound (117 mg).

後処理

  1. additionwas added to the reaction solution at room temperature
  2. concentrationat room temperature, and the obtained mixture was then concentrated under a reduced pressure
  3. additionDiethyl ether was added to the residue for solidification
  4. temperaturewhile cooling on ice
  5. filtrationa solid was then collected by filtration
  6. washThe solid was washed with diethyl ether

出典と根拠

ORDレコード
ord-53d0ce7923fb4321bddd80abb534aa47
出典データセット
uspto-grants-2009_05
特許番号
US07538123B2

反応ノート

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