Methyl iodide → HCID 21555000、化合物

HRID 267551ノート

反応式

HRID 267551 の反応式
[CH2:1]1[CH:16]2[N:4]([CH2:5][CH2:6][C:7]3[C:15]4[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=4)[NH:9][C:8]=32)[CH2:3][CH2:2]1.[H-].[Na+].[CH3:19]I>CN(C)C=O>[CH3:19][N:9]1[C:10]2[C:15](=[CH:14][CH:13]=[CH:12][CH:11]=2)[C:7]2[CH2:6][CH2:5][N:4]3[CH:16]([C:8]1=2)[CH2:1][CH2:2][CH2:3]3

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 372331NSC647389

生成物 1

HCID 21555000HCID 21555000、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
25 °C

実験手順

2,3,5,6,11,11b-Hexahydro-1H-indolizino[8,7-b]-indole (8.49 g.) is stirred for 1 hour at 25°C. in dimethylformamide (200 ml.) containing sodium hydride (2.11 g. of a 50% mineral oil dispersion). Methyl iodide (6.25 g.) in dimethylformamide (25 ml.) is added and the mixture is stirred at 25°C. for 16 hours. The dimethylformamide is distilled off, and the residue is dissolved in chloroform and washed with aqueous potassium bicarbonate and water, and dried. The product is chromatographed on neutral alumina to give 2,3,5,6,11,11b-hexahydro-11-methyl-1H-indolizino[8,7-b]indole as a clear oil (5.88 g.).

後処理

  1. distillationThe dimethylformamide is distilled off
  2. dissolutionthe residue is dissolved in chloroform
  3. washwashed with aqueous potassium bicarbonate and water
  4. customdried
  5. customThe product is chromatographed on neutral alumina

出典と根拠

ORDレコード
ord-e59f2ff5d65e46b3bcd979769ed95266
出典データセット
uspto-grants-1976_03
特許番号
US03943148

反応ノート

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