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Benzyl Bromide → 1-Benzyl-2-carboethoxy-4-methoxy-6,7,8,9-tetrahydro-1h-benz[g]indole

HRID 489109
ノート
印刷プレビュー

反応式

HRID 489109 の反応式
[H-].[Na+].[C:3]([C:8]1[NH:9][C:10]2[C:15]([CH:16]=1)=[C:14]([O:17][CH3:18])[CH:13]=[C:12]1[CH2:19][CH2:20][CH2:21][CH2:22][C:11]=21)([O:5][CH2:6][CH3:7])=[O:4].[CH2:23](Br)[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1>O>[CH2:23]([N:9]1[C:10]2[C:15](=[C:14]([O:17][CH3:18])[CH:13]=[C:12]3[CH2:19][CH2:20][CH2:21][CH2:22][C:11]3=2)[CH:16]=[C:8]1[C:3]([O:5][CH2:6][CH3:7])=[O:4])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 7498Benzyl Bromide2 回HCID 24758Sodium hydride2 回HCID 111848862-Carboethoxy-4-methoxy-6,7,8,9-tetrahydro-1h-benz[g]indole

生成物 1

HCID 112106971-Benzyl-2-carboethoxy-4-methoxy-6,7,8,9-tetrahydro-1h-benz[g]indole収率 37.4%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A suspension of 60% sodium hydride in mineral oil (4.08 g, 0.102 mol) was washed once with hexane and suspended in dry N,N-dimethylformamide (100 mL). 2-Carboethoxy-4-methoxy-6,7,8,9-tetrahydro-1H-benz[g]indole (25.4 g, 92.7 mmol) was added in several portions resulting in gas evolution. Benzyl bromide (12.1 mL, 102 mmol) was added in two portions over 30 min and the resulting mixture stirred for 18 h. Additional portions of 60% sodium hydride suspension (1.30 g) and benzyl bromide (2 mL) were added and the mixture stirred for 27 h. The mixture was poured into water (2 L) and the resulting solution extracted three times with ethyl acetate. The combined extracts were Washed three times with water, dried (sodium sulfate), filtered, and concentrated in vacuo. Chromatography (silica gel) provided 12.6 g (37%) of the title compound as a yellow solid: mp 86-88° C. 1H NMR (CDCl3) δ 7.51 (s, 1H), 7.20 (m, 3H), 6.84 (d, J=6.6 Hz, 2H), 6.24 (s, 1H), 6.12 (s, 2H), 4.23 (q, J=7.0 Hz, 2H), 3.93 (s, 3H), 2.96 (m, 2H), 2.85 (m, 2H), 1.71 (m, 4H), 1.30 (t, J=7.0 Hz, 3H); MS ES+ m/e 364 (p+1); IR (CHCl3, cm−1) 2937, 1701, 1502.

後処理

  1. washwas washed once with hexane
  2. customresulting in gas evolution
  3. stirringthe mixture stirred for 27 h
  4. extractionthe resulting solution extracted three times with ethyl acetate
  5. washThe combined extracts were Washed three times with water
  6. dry with materialdried (sodium sulfate)
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-3b396431952d4a09b2d491a864f30453
出典データセット
uspto-grants-2005_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06974831B2

反応ノート

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