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

HRID 2237586

反応式

HRID 2237586 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.[CH2:31]([S:33](O)(=[O:35])=[O:34])[CH3:32]>CC(C)CC(=O)C>[CH2:31]([S:33]([O:28][C@@H:14]1[CH2:13][CH2:12][C@@H:11]2[C@@H:16]([C:17]3[C:22]([C:9]([C:8]4[C:3]([O:2][CH3:1])=[N:4][C:5]([O:29][CH3:30])=[CH:6][CH:7]=4)=[N:10]2)=[CH:21][C:20]([O:23][CH3:24])=[C:19]([O:25][CH2:26][CH3:27])[CH:18]=3)[CH2:15]1)(=[O:35])=[O:34])[CH3:32]

参加物

4

反応物 2

HCID 11668Ethanesulfonic acidHCID 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 91044709(2R,4aR,10bR)-6-(2,6-Dimethoxy-pyridin-3-yl)-9-ethoxy-8-methoxy-1,2,3,4,4a, 10b-hexahydro-phenanthridin-2-ol ethansulfonate収率 96.9%

試薬・触媒・溶媒 1

HCID 7909Methyl Isobutyl Ketone溶媒

反応条件

温度
50 °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 (1.5 g; 3.64 mmol) is dissolved in 9 ml of 4-methyl-2-pentanone. The solution is heated up to 50° C. 312 μl (3.82 mmol) of ethansulfonic acid are added. After crystallisation 3 ml 4-methyl-2-pentanon is added and the suspension is stirred over night. The crystals are filtered off and dried to obtain 1.78 g (94%) of the title compound (m.p.: 216° C.).

後処理

  1. customAfter crystallisation 3 ml 4-methyl-2-pentanon
  2. additionis added
  3. filtrationThe crystals are filtered off
  4. customdried

出典と根拠

ORDレコード
ord-2892eebb22a24ed89c6adfc4926ecf8e
出典データセット
uspto-grants-2010_05
特許番号
US07718668B2

関連ノート

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