Methyl iodide → HCID 21555000, 화합물

HRID 267551노트

반응식

HRID 267551 반응식
[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

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 372331NSC647389

생성물 1

HCID 21555000HCID 21555000, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

반응 조건

온도
25 °C

실험 절차

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.).

후처리

  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

출처 및 근거

ORD 기록
ord-e59f2ff5d65e46b3bcd979769ed95266
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03943148

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