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

HRID 728736

反応式

HRID 728736 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+].C[C:29]([CH3:31])=[O:30]>>[ClH:1].[N:2]1([CH2:7][CH:8]([N:10]2[C:23]3[CH:22]=[C:31]([C:29]([OH:26])=[O:30])[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

4

反応物 3

HCID 180AcetoneHCID 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

実験手順

10-[1-(1-Pyrrolidinyl)-2-propyl]-2-phenothiazinecarbonitrile hydrochloride, L series (5 g) is added to a solution of potassium hydroxide (1.75 g) in glycol (30 cc), and the mixture is stirred for 4 hours under reflux. After being cooled, the yellow solution obtained is diluted with acetone (75 cc) and a 3N solution (5 cc) of hydrochloric acid in ethyl ether, filtered and diluted again with acetone (75 cc) and a 3N solution (5 cc) of hydrochloric acid in ethyl ether. After priming, the mixture is left to crystallize for 16 hours at a temperature in the region of 5° C. The solid obtained is drained, washed with ethyl ether (10 cc) and dried under reduced pressure (5 mm Hg; 0.7 kPa) at 40° C. 10-[1-(1-Pyrrolidinyl)-2-propyl]-2-phenothiazinecarboxylic acid hydrochloride, L series (2.9 g) is thereby obtained in the form of a pale yellow solid, m.p. 200-210° C. (melts forming a paste).

後処理

  1. temperatureunder reflux
  2. temperatureAfter being cooled
  3. customthe yellow solution obtained
  4. filtrationa 3N solution (5 cc) of hydrochloric acid in ethyl ether, filtered
  5. additiondiluted again with acetone (75 cc)
  6. waitthe mixture is left
  7. customto crystallize for 16 hours at a temperature in the region of 5° C
  8. customThe solid obtained
  9. washwashed with ethyl ether (10 cc)
  10. customdried under reduced pressure (5 mm Hg; 0.7 kPa) at 40° C

出典と根拠

ORDレコード
ord-a03ba0586480441ca73b9ade375d8855
出典データセット
uspto-grants-1991_09
特許番号
US05049669

関連ノート

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