Fumaric Acid → N-(2-Hydroxybenzyl)-10-[(2RS)-1-(1-pyrrolidinyl)-2-propyl]-2-phenothiazinecarboxamide fumarate

HRID 704243ノート

反応式

HRID 704243 の反応式
[OH:1][C:2]1[CH:33]=[CH:32][CH:31]=[CH:30][C:3]=1[CH2:4][NH:5][C:6]([C:8]1[CH:21]=[CH:20][C:19]2[S:18][C:17]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[N:11]([CH:22]([CH3:29])[CH2:23][N:24]3[CH2:28][CH2:27][CH2:26][CH2:25]3)[C:10]=2[CH:9]=1)=[O:7].[C:34]([OH:41])(=[O:40])/[CH:35]=[CH:36]/[C:37]([OH:39])=[O:38]>CC(O)C>[C:34]([OH:41])(=[O:40])/[CH:35]=[CH:36]/[C:37]([OH:39])=[O:38].[OH:1][C:2]1[CH:33]=[CH:32][CH:31]=[CH:30][C:3]=1[CH2:4][NH:5][C:6]([C:8]1[CH:21]=[CH:20][C:19]2[S:18][C:17]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[N:11]([CH:22]([CH3:29])[CH2:23][N:24]3[CH2:25][CH2:26][CH2:27][CH2:28]3)[C:10]=2[CH:9]=1)=[O:7]

参加物

4

反応物 2

HCID 444972Fumaric AcidHCID 20074856N-(2-hydroxybenzyl)-10-[(2RS)-1-(1-pyrrolidinyl)-2-propyl]-2-phenothiazinecarboxamide

生成物 1

HCID 20074855N-(2-Hydroxybenzyl)-10-[(2RS)-1-(1-pyrrolidinyl)-2-propyl]-2-phenothiazinecarboxamide fumarate収率 46.8%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒2 回

実験手順

N-(2-Hydroxybenzyl)-10-[(2RS)-1-(1-pyrrolidinyl)-2-propyl]-2-phenothiazinecarboxamide (1.86 g) is dissolved in boiling 2-propanol (22 cc). A solution of fumaric acid (0.47 g) in 2-propanol (18 cc) under reflux is added to this solution. After cooling, the crystals formed are washed with ethyl ether (2×10 cc), filtered and dried under reduced pressure (5 mm Hg; 0.67 kPa) at 50° C. N-(2-Hydroxybenzyl)-10-[(2RS)-1-(1-pyrrolidinyl)-2-propyl]-2-phenothiazinecarboxamide fumarate (1.09 g) is thereby obtained in the form of yellow crystals, m.p. about 80° C.

後処理

  1. additionis added to this solution
  2. temperatureAfter cooling
  3. customthe crystals formed
  4. washare washed with ethyl ether (2×10 cc)
  5. filtrationfiltered
  6. customdried under reduced pressure (5 mm Hg; 0.67 kPa) at 50° C

出典と根拠

ORDレコード
ord-f2e34afa41c24fd883f98e7f27bbb8f0
出典データセット
uspto-grants-1991_01
特許番号
US04985419

反応ノート

読み込み中…