1-Acetyl-7-(1-methylpiperidin-4-yl)-1,2,3,5-tetrahydropyrrolo[2,3-f]indole → 7-(1-Methylpiperidin-4-yl)-1,2,3,5-tetrahydropyrrolo[2,3-f]indole

HRID 1936710

反応式

HRID 1936710 の反応式
C([N:4]1[C:8]2=[CH:9][C:10]3[C:11]([CH:16]4[CH2:21][CH2:20][N:19]([CH3:22])[CH2:18][CH2:17]4)=[CH:12][NH:13][C:14]=3[CH:15]=[C:7]2[CH2:6][CH2:5]1)(=O)C>C(O)C.[OH-].[Na+].O>[CH3:22][N:19]1[CH2:20][CH2:21][CH:16]([C:11]2[C:10]3[CH:9]=[C:8]4[NH:4][CH2:5][CH2:6][C:7]4=[CH:15][C:14]=3[NH:13][CH:12]=2)[CH2:17][CH2:18]1

参加物

5

反応物 1

HCID 224625471-Acetyl-7-(1-methylpiperidin-4-yl)-1,2,3,5-tetrahydropyrrolo[2,3-f]indole

生成物 1

HCID 178989527-(1-Methylpiperidin-4-yl)-1,2,3,5-tetrahydropyrrolo[2,3-f]indole収率 61.4%

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒HCID 962Water溶媒HCID 14798Sodium Hydroxide溶媒2 回

実験手順

To a stirred suspension of 1-acetyl-7-(1-methylpiperidin-4-yl)-1,2,3,5-tetrahydropyrrolo[2,3-f]indole (D5, 0.55 g, 1.85 mmole) in ethanol (10 ml) and 10% sodium hydroxide solution (10 ml) was added sodium hydroxide pellets (0.50 g) and the resultant mixture was heated at reflux under argon for 18 hours. The mixture was cooled, diluted with water (75 ml) and extracted with dichloromethane (5×30 ml). The combined organic extracts were washed with brine, dried (MgSO4) and evaporated to dryness. The residue was triturated with diethyl ether and the solid filtered off and dried in vacuo to afford the title compound as an off-white powder (0.29 g).

後処理

  1. temperatureat reflux under argon for 18 hours
  2. temperatureThe mixture was cooled
  3. extractionextracted with dichloromethane (5×30 ml)
  4. washThe combined organic extracts were washed with brine
  5. dry with materialdried (MgSO4)
  6. customevaporated to dryness
  7. customThe residue was triturated with diethyl ether
  8. filtrationthe solid filtered off
  9. customdried in vacuo

出典と根拠

ORDレコード
ord-5b3a5230f34840c1bdb1304e9a1eca36
出典データセット
uspto-grants-2002_05
特許番号
US06391891B1

関連ノート

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