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

HRID 728736
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HRID 728736 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

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

생성물 1

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

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-a03ba0586480441ca73b9ade375d8855
출처 데이터셋
uspto-grants-1991_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05049669

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