Water → HCID 135816654、化合物

HRID 1493174ノート

反応式

HRID 1493174 の反応式
[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]

参加物

6

反応物 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 516892Sodium BicarbonateHCID 15020700HCID 15020700、化合物

生成物 1

HCID 135816654HCID 135816654、化合物収率 47.9%

試薬・触媒・溶媒 1

HCID 260Hydrogen Bromide溶媒

反応条件

温度
120 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-fa61085517bf472d93110015086b9c31
出典データセット
uspto-grants-1991_06
特許番号
US05021421

反応ノート

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