Acetone → 10-[1-(1-Pyrrolidinyl)-2-propyl]-2-phenothiazinecarboxylic acid hydrochloride

HRID 704238

反応式

HRID 704238 の反応式
[ClH:1].[N:2]1([CH2:7][CH:8]([N:10]2[C:23]3[CH:22]=C(C#N)[CH:20]=[CH:19][C:18]=3[S:17][C:16]3[C:11]2=[CH:12][CH:13]=[CH:14][CH:15]=3)[CH3:9])[CH2:6][CH2:5][CH2:4][CH2:3]1.[OH-:26].[K+].Cl.C[C:30]([CH3:32])=[O:31]>C(OCC)C>[ClH:1].[N:2]1([CH2:7][CH:8]([N:10]2[C:23]3[CH:22]=[C:32]([C:30]([OH:26])=[O:31])[CH:20]=[CH:19][C:18]=3[S:17][C:16]3[C:11]2=[CH:12][CH:13]=[CH:14][CH:15]=3)[CH3:9])[CH2:6][CH2:5][CH2:4][CH2:3]1

参加物

6

反応物 4

HCID 180AcetoneHCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 1902054310-[1-(1-Pyrrolidinyl)-2-propyl]-2-phenothiazinecarbonitrile hydrochloride

生成物 1

HCID 1453664010-[1-(1-Pyrrolidinyl)-2-propyl]-2-phenothiazinecarboxylic acid hydrochloride

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

10-[(2RS)-1-(1-Pyrrolidinyl)-2-propyl]-2-phenothiazinecarbonitrile hydrochloride (3.72 g) is added to a solution of potassium hydroxide (1.7 g) in glycol (20 cc), and the mixture is stirred for 5 hours under reflux. After cooling, the yellow solution obtained is traeted with a 3N ethereal solution (10 cc) of hydrochloric acid, and diluted with acetone (100 cc) and ethyl ether (100 cc) and then filtered. The yellow filtrate, after priming, gives rise to the crystallization of a product, which is drained, washed with ethyl ether (2×10 cc) and dried under reduced pressure (5 mm Hg; 0.68 kPa) at 40° C. 10-[(2RS)-1-(1-Pyrrolidinyl)-2-propyl]-2-phenothiazinecarboxylic acid hydrochloride (3.5 g) is thereby obtained in the form of pale yellow crystals, m.p. 215°-217° C.

後処理

  1. temperatureunder reflux
  2. temperatureAfter cooling
  3. customthe yellow solution obtained
  4. filtrationfiltered
  5. customThe yellow filtrate, after priming, gives rise
  6. customto the crystallization of a product, which
  7. washwashed with ethyl ether (2×10 cc)
  8. customdried under reduced pressure (5 mm Hg; 0.68 kPa) at 40° C

出典と根拠

ORDレコード
ord-6e575cacd2934a42b2707d859b388d67
出典データセット
uspto-grants-1991_01
特許番号
US04985419

関連ノート

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