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

HRID 55384노트

반응식

HRID 55384 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a4b0db77e7704429b9a2a0480f4d84fc
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05624961

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