Water → HCID 135816654, 화합물

HRID 1493174노트

반응식

HRID 1493174 반응식
[CH2:1]([N:3]1[CH2:8][CH2:7][N:6]([C:9]2[N:14]=[C:13]3[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][C:12]3=[C:11]([C:21]3[CH:26]=[CH:25][C:24]([O:27]C)=[CH:23][CH:22]=3)[CH:10]=2)[CH2:5][CH2:4]1)[CH3:2].O.[OH-].[Na+].C(=O)([O-])O.[Na+]>Br>[CH2:1]([N:3]1[CH2:8][CH2:7][N:6]([C:9]2[N:14]=[C:13]3[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][C:12]3=[C:11]([C:21]3[CH:26]=[CH:25][C:24]([OH:27])=[CH:23][CH:22]=3)[CH:10]=2)[CH2:5][CH2:4]1)[CH3:2]

참가 물질

6

반응물 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 516892Sodium BicarbonateHCID 15020700HCID 15020700, 화합물

생성물 1

HCID 135816654HCID 135816654, 화합물수율 47.9%

시약·촉매·용매 1

HCID 260Hydrogen Bromide용매

반응 조건

온도
120 °C

실험 절차

2-(4-Ethyl-1-piperazinyl)-4-(4-methoxyphenyl)-5,6,7,8,9,10-hexahydrocycloocta[b]pyridine (1.3 g) is dissolved in 48% hydrobromic acid (10 ml) and the mixture is stirred at 120° C. for 2 hours. After cooling, water is added thereto and the mixture is neutralized with 1N aqueous sodium hydroxide solution and sodium hydrogen carbonate. The resulting precipitate is collected by filtration, washed with water, and recrystallized from methanol to give the desired product (0.6 g), m.p. 250°-253° C.

후처리

  1. temperatureAfter cooling
  2. filtrationThe resulting precipitate is collected by filtration
  3. washwashed with water
  4. customrecrystallized from methanol

출처 및 근거

ORD 기록
ord-fa61085517bf472d93110015086b9c31
출처 데이터셋
uspto-grants-1991_06
특허 번호
US05021421

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