Triethylamine → N-(3-hydroxy-6-methoxy-2,4,5-trimethylbenzyl)-2-(4-acetylamino-2-isopropyl-5-methylphenoxy)ethylamine

HRID 55384ノート

反応式

HRID 55384 の反応式
[C:1]([NH:4][C:5]1[C:14]([CH3:15])=[CH:13][C:8]([O:9][CH2:10][CH2:11][NH2:12])=[C:7]([CH:16]([CH3:18])[CH3:17])[CH:6]=1)(=[O:3])[CH3:2].C(N(CC)CC)C.[OH:26][C:27]1[C:28]([CH3:39])=[C:29]([C:32]([O:37][CH3:38])=[C:33]([CH3:36])[C:34]=1[CH3:35])[CH2:30]Cl>CN(C)C=O>[OH:26][C:27]1[C:28]([CH3:39])=[C:29]([C:32]([O:37][CH3:38])=[C:33]([CH3:36])[C:34]=1[CH3:35])[CH2:30][NH:12][CH2:11][CH2:10][O:9][C:8]1[CH:13]=[C:14]([CH3:15])[C:5]([NH:4][C:1](=[O:3])[CH3:2])=[CH:6][C:7]=1[CH:16]([CH3:18])[CH3:17]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 109218743-Hydroxy-6-methoxy-2,4,5-trimethylbenzyl chlorideHCID 199577142-(4-Acetylamino-2-isopropyl-5-methylphenoxy)ethylamine

生成物 1

HCID 19957661N-(3-hydroxy-6-methoxy-2,4,5-trimethylbenzyl)-2-(4-acetylamino-2-isopropyl-5-methylphenoxy)ethylamine収率 5.8%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

2-(4-Acetylamino-2-isopropyl-5-methylphenoxy)ethylamine (1.0 g) and triethylamine (0.50 g) were dissolved in N,N-dimethylformamide (20 ml), and 3-hydroxy-6-methoxy-2,4,5-trimethylbenzyl chloride (0.86 g) dissolved in N,N-dimethylformamide (10 ml) was added dropwise while stirring the mixture at room temperature. The mixture was stirred for 5 hours. After the completion of the reaction, the solvent was distilled off, and water and ethyl acetate were added. The mixture was stirred and an insoluble matter was collected by filtration. The obtained solid was recrystallized from ethyl acetate to give 100 mg of the title compound.

後処理

  1. additionwas added dropwise
  2. stirringThe mixture was stirred for 5 hours
  3. customAfter the completion of the reaction
  4. distillationthe solvent was distilled off
  5. additionwater and ethyl acetate were added
  6. stirringThe mixture was stirred
  7. filtrationan insoluble matter was collected by filtration
  8. customThe obtained solid was recrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-a4b0db77e7704429b9a2a0480f4d84fc
出典データセット
uspto-grants-1997_04
特許番号
US05624961

反応ノート

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