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Acetic Acid → HCID 18001088、化合物

HRID 1870452
ノート
印刷プレビュー

反応式

HRID 1870452 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([C:12](=[O:22])[CH:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]3([O:20][CH3:21])N)[CH2:10][CH2:9][CH2:8][CH:7]([CH2:23][C:24]([N:26]3[CH2:31][CH2:30][N:29]([CH3:32])[CH2:28][CH2:27]3)=[O:25])[C:6]=2[CH:33]=1.[C:34]1([CH3:42])[C:35]([CH:40]=O)=[CH:36][CH:37]=[CH:38][CH:39]=1.C(O)(=O)C.C([BH3-])#[N:48].[Na+]>CO>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([C:12](=[O:22])[C:13]3[CH:18]=[CH:17][C:16]([NH:48][CH2:40][C:35]4[CH:36]=[CH:37][CH:38]=[CH:39][C:34]=4[CH3:42])=[CH:15][C:14]=3[O:20][CH3:21])[CH2:10][CH2:9][CH2:8][CH:7]([CH2:23][C:24]([N:26]3[CH2:27][CH2:28][N:29]([CH3:32])[CH2:30][CH2:31]3)=[O:25])[C:6]=2[CH:33]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 176Acetic AcidHCID 107222-MethylbenzaldehydeHCID 5003444Sodium cyanoborohydrideHCID 18001077HCID 18001077、化合物

生成物 1

HCID 18001088HCID 18001088、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
55 °C

実験手順

To a solution of 7-chloro-5-[(4-methyl-1-piperazinyl)carbonyl-methyl]-1-(2-methoxy-2-aminobenzoyl)-2,3,4,5-tetrahydro-1H-benzazepine (0.8 g) in methanol (30 ml) are added o-tolualdehyde (0.35 ml) and acetic acid (1 ml), and the mixture is stirred at 50-60° C. for 2-3 hours. To the mixture is added sodium cyanoborohydride (0.11 g) at room temperature, and the mixture is stirred for two hours. The mixture is evaporated to remove the solvent, and to the residue is added water. The mixture is extracted with ethyl acetate, and the extract is dried, and evaporated. The residue is purified by silica gel column chromatography (solvent; dichloromethane:methanol =50:1→25:1), and recrystallized from acetone/diethyl ether to give 7-chloro-5-[(4-methyl-1-piperazinyl)carbonylmethyl]-1-[2-methoxy-4-(2-methylbenzylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzazepine (0.71 g) as white powder.

後処理

  1. stirringthe mixture is stirred for two hours
  2. customThe mixture is evaporated
  3. customto remove the solvent
  4. additionto the residue is added water
  5. extractionThe mixture is extracted with ethyl acetate
  6. customthe extract is dried
  7. customevaporated
  8. customThe residue is purified by silica gel column chromatography (solvent; dichloromethane:methanol =50:1→25:1)
  9. customrecrystallized from acetone/diethyl ether

出典と根拠

ORDレコード
ord-097102e3e66e4888bc7e1aa3f459234c
出典データセット
uspto-grants-2000_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06096735

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート