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1-[7,8-Dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-on-3-yl]-3-[N-benzyl-N-(6,7-dimethoxy-1,2,3,4-tetrahydronaphth-2-yl)-amino]-propane → 1-[7,8-Dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-on-3-yl]-3-[N-(6,7-dimethoxy-1,2,3,4-tetrahydronaphth-2-yl)-amino]-propane

HRID 1380883
ノート
印刷プレビュー

反応式

HRID 1380883 の反応式
[CH3:1][O:2][C:3]1[C:39]([O:40][CH3:41])=[CH:38][C:6]2[CH2:7][C:8](=[O:37])[N:9]([CH2:12][CH2:13][CH2:14][N:15](CC3C=CC=CC=3)[CH:16]3[CH2:25][CH2:24][C:23]4[C:18](=[CH:19][C:20]([O:28][CH3:29])=[C:21]([O:26][CH3:27])[CH:22]=4)[CH2:17]3)[CH2:10][CH2:11][C:5]=2[CH:4]=1>C(O)(=O)C.[Pd]>[CH3:1][O:2][C:3]1[C:39]([O:40][CH3:41])=[CH:38][C:6]2[CH2:7][C:8](=[O:37])[N:9]([CH2:12][CH2:13][CH2:14][NH:15][CH:16]3[CH2:25][CH2:24][C:23]4[C:18](=[CH:19][C:20]([O:28][CH3:29])=[C:21]([O:26][CH3:27])[CH:22]=4)[CH2:17]3)[CH2:10][CH2:11][C:5]=2[CH:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 135796501-[7,8-Dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-on-3-yl]-3-[N-benzyl-N-(6,7-dimethoxy-1,2,3,4-tetrahydronaphth-2-yl)-amino]-propane

生成物 1

HCID 135796591-[7,8-Dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-on-3-yl]-3-[N-(6,7-dimethoxy-1,2,3,4-tetrahydronaphth-2-yl)-amino]-propane

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 176Acetic Acid溶媒

実験手順

Here, 1-[7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-on-3-yl]-3-[N-benzyl-N-(6,7-dimethoxy-1,2,3,4-tetrahydronaphth-2-yl)-amino]-propane (0.78 g, 0.0014 mol) is hydrogenated in glacial acetic acid (20 ml) in the presence of 10% palladium/charcoal (0.1 g) for 3 hours at ambient temperature under pressure (5 bar). The catalyst is removed by suction filtering, the glacial acetic acid is distilled off in vacuo, the residue is taken up in methylene chloride/saturated potassium carbonate solution, the organic phase is washed with water, dried over magnesium sulphate, evaporated again and purified over alumina (100 g), neutral, activity II, with methylene chloride and then with increasing amounts of ethanol (up to 40%). The hydrochloride is precipitated from a solution in acetone with ethereal hydrochloric acid. Yield: 0.45 g Mp: 222°-223° C.

後処理

  1. customThe catalyst is removed by suction
  2. filtrationfiltering
  3. distillationthe glacial acetic acid is distilled off in vacuo
  4. washthe organic phase is washed with water
  5. dry with materialdried over magnesium sulphate
  6. customevaporated again
  7. custompurified over alumina (100 g)
  8. customThe hydrochloride is precipitated from a solution in acetone with ethereal hydrochloric acid

出典と根拠

ORDレコード
ord-ecdb55d6932641d3b460980477c2d47a
出典データセット
uspto-grants-1986_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04584293

反応ノート

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