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Fumaric Acid → HCID 20074838、化合物

HRID 704206
ノート
印刷プレビュー

反応式

HRID 704206 の反応式
[C:1]([OH:8])(=[O:7])/[CH:2]=[CH:3]/[C:4]([OH:6])=[O:5].[CH:9]1([CH2:13][NH:14][C:15]([C:17]2[CH:30]=[CH:29][C:28]3[S:27][C:26]4[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=4)[N:20]([CH:31]([CH3:38])[CH2:32][N:33]4[CH2:37][CH2:36][CH2:35][CH2:34]4)[C:19]=3[CH:18]=2)=[S:16])[CH2:12][CH2:11][CH2:10]1>CC(O)C>[C:1]([OH:8])(=[O:7])/[CH:2]=[CH:3]/[C:4]([OH:6])=[O:5].[CH:9]1([CH2:13][NH:14][C:15]([C:17]2[CH:30]=[CH:29][C:28]3[S:27][C:26]4[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=4)[N:20]([CH:31]([CH3:38])[CH2:32][N:33]4[CH2:34][CH2:35][CH2:36][CH2:37]4)[C:19]=3[CH:18]=2)=[S:16])[CH2:12][CH2:11][CH2:10]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 444972Fumaric AcidHCID 20074839HCID 20074839、化合物

生成物 1

HCID 20074838HCID 20074838、化合物

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒2 回

実験手順

A solution of fumaric acid (0.58 g) in 2-propanol (14 cc) under reflux is added to a solution of N-cyclobutylmethyl-10-[1-(1-pyrrolidinyl)-2-propyl]-2-phenothiazinecarbothioamide, L series (2.19 g) in 2-propanol (16 cc) under reflux. After cooling, the mixture is concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C. and the residue is taken up with stirring for 16 hours with isopropyl ether (70 cc). The suspension obtained is filtered and the solid is dried under reduced pressure (5 mm Hg; 4 kPa) at 50° C. and dissolved in 2-propanol under reflux (50 cc). After cooling, the product crystallizes and stirring is continued for 16 hours at 20° C. The crystals are filtered off and dried under reduced pressure (5 mm Hg; 4 kPa) at 50° C. N-Cyclobutylmethyl-10-[1-(1-pyrrolidinyl)-2-propyl]-2-phenothiazinecarbothioamide fumarate, L series (1.52 g) is thereby obtained in the form of yellow crystals, m.p. 194° C.

後処理

  1. temperatureunder reflux
  2. temperatureAfter cooling
  3. concentrationthe mixture is concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C.
  4. customThe suspension obtained
  5. filtrationis filtered
  6. customthe solid is dried under reduced pressure (5 mm Hg; 4 kPa) at 50° C.
  7. dissolutiondissolved in 2-propanol
  8. temperatureunder reflux (50 cc)
  9. temperatureAfter cooling
  10. customthe product crystallizes
  11. stirringstirring
  12. waitis continued for 16 hours at 20° C
  13. filtrationThe crystals are filtered off
  14. customdried under reduced pressure (5 mm Hg; 4 kPa) at 50° C

出典と根拠

ORDレコード
ord-b2bbfd926fcb4b6bbf6b2002bb464bfa
出典データセット
uspto-grants-1991_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04985419

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート