Hydrogen Bromide → (2R,4aR,10bR)-6-(2,6-Dimethoxy-pyridin-3-yl)-9-ethoxy-8-methoxy-1,2,3,4,4a,10b-hexahydro-phenanthridin-2-ol hydrobromide

HRID 406942

反応式

HRID 406942 の反応式
[CH3:1][O:2][C:3]1[C:8]([C:9]2[C:22]3[C:17](=[CH:18][C:19]([O:25][CH2:26][CH3:27])=[C:20]([O:23][CH3:24])[CH:21]=3)[C@@H:16]3[C@@H:11]([CH2:12][CH2:13][C@@H:14]([OH:28])[CH2:15]3)[N:10]=2)=[CH:7][CH:6]=[C:5]([O:29][CH3:30])[N:4]=1.[BrH:31]>CC(C)CC(=O)C>[BrH:31].[CH3:1][O:2][C:3]1[C:8]([C:9]2[C:22]3[C:17](=[CH:18][C:19]([O:25][CH2:26][CH3:27])=[C:20]([O:23][CH3:24])[CH:21]=3)[C@@H:16]3[C@@H:11]([CH2:12][CH2:13][C@@H:14]([OH:28])[CH2:15]3)[N:10]=2)=[CH:7][CH:6]=[C:5]([O:29][CH3:30])[N:4]=1

参加物

4

反応物 2

HCID 260Hydrogen BromideHCID 11258441(2R,4aR,10bR)-6-(2,6-Dimethoxy-pyridin-3-yl)-9-ethoxy-8-methoxy-1,2,3,4,4a,10b-hexahydro-phenanthridin-2-ol

生成物 1

HCID 67022669(2R,4aR,10bR)-6-(2,6-Dimethoxy-pyridin-3-yl)-9-ethoxy-8-methoxy-1,2,3,4,4a,10b-hexahydro-phenanthridin-2-ol hydrobromide収率 97%

試薬・触媒・溶媒 1

HCID 7909Methyl Isobutyl Ketone溶媒

反応条件

温度
60 °C

実験手順

(2R,4aR,10bR)-6-(2,6-Dimethoxy-pyridin-3-yl)-9-ethoxy-8-methoxy-1,2,3,4,4a,10b-hexahydro-phenanthridin-2-ol (1.2 g; 2.9 mmol) is dissolved in 7.2 ml of 4-methyl-2-pentanone. The solution is heated up to 60° C. 350 μl (3.05 mmol) of aqueous HBr (W=47%) are added. After crystallisation the suspension is stirred over night. The crystals are filtered off and dried to obtain 1.38 g (97%) of the title compound (m.p.: 163° C.).

後処理

  1. customAfter crystallisation the suspension
  2. filtrationThe crystals are filtered off
  3. customdried

出典と根拠

ORDレコード
ord-a8cd826a849c4e509d6f6f90ee3790e1
出典データセット
uspto-grants-2014_06
特許番号
US08754218B2

関連ノート

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