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Hydrochloric Acid → 4-[(4-Hydroxy-4-n-octyl)cyclohexylamino]-3-methoxy-2-methylpyridine

HRID 1009
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반응식

HRID 1009 반응식
[Mg].[CH2:2](Br)[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH3:9].O=[C:12]1[CH2:17][CH2:16][CH:15]([NH:18][C:19]2[CH:24]=[CH:23][N:22]=[C:21]([CH3:25])[C:20]=2[O:26][CH3:27])[CH2:14][CH2:13]1.Cl.C1C[O:32]CC1>>[OH:32][C:5]([N:18]([CH:15]1[CH2:16][CH2:17][CH2:12][CH2:13][CH2:14]1)[C:19]1[CH:24]=[CH:23][N:22]=[C:21]([CH3:25])[C:20]=1[O:26][CH3:27])([CH2:6][CH2:7][CH2:8][CH3:9])[CH2:4][CH2:3][CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 5

HCID 313Hydrochloric AcidHCID 8028Tetrahydrofuran2회HCID 81401-BromooctaneHCID 5462224MagnesiumHCID 196939514-(4-Oxocyclohexylamino)-3-methoxy-2-methylpyridine

생성물 1

HCID 677539694-[(4-Hydroxy-4-n-octyl)cyclohexylamino]-3-methoxy-2-methylpyridine

실험 절차

The Grignard solution is prepared from 0.73 g of magnesium and 6.0 g of octyl bromide in 50 ml of absolute THF. 2.8 g of 4-(4-oxocyclohexylamino)-3-methoxy-2-methylpyridine in 20 ml of THF are added dropwise to the solution. After 2 hours the mixture is acidified with 2N HCl. The THF is then distilled off in vacuo at room temperature and the product is extracted from the solution which is rendered alkaline with methylene chloride. Further working up takes place as in the previous working procedure.

후처리

  1. distillationThe THF is then distilled off in vacuo at room temperature
  2. extractionthe product is extracted from the solution which

출처 및 근거

ORD 기록
ord-8babbf86aa35457596df795b424dbf27
출처 데이터셋
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05723450

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