Hydrochloric Acid → 4-({3-[4-(Phenylcarbonyl)piperazin-1-yl]azetidin-1-yl}carbonyl)phenol

HRID 1852608노트

반응식

HRID 1852608 반응식
C([O:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]([N:13]2[CH2:16][CH:15]([N:17]3[CH2:22][CH2:21][N:20]([C:23]([C:25]4[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=4)=[O:24])[CH2:19][CH2:18]3)[CH2:14]2)=[O:12])=[CH:7][CH:6]=1)(=O)C.[Li+].[OH-].Cl>C1COCC1.CO.O>[C:25]1([C:23]([N:20]2[CH2:21][CH2:22][N:17]([CH:15]3[CH2:16][N:13]([C:11]([C:8]4[CH:7]=[CH:6][C:5]([OH:4])=[CH:10][CH:9]=4)=[O:12])[CH2:14]3)[CH2:18][CH2:19]2)=[O:24])[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 596259394-({3-[4-(Phenylcarbonyl)piperazin-1-yl]azetidin-1-yl}carbonyl)phenyl acetate

생성물 1

HCID 596258104-({3-[4-(Phenylcarbonyl)piperazin-1-yl]azetidin-1-yl}carbonyl)phenol

시약·촉매·용매 1

HCID 21892291Methanol tetrahydrofuran water용매

실험 절차

A mixture of compound 26c (420 mg, 1.03 mmol) and LiOH (100 mg, 4.0 mmol) in a solvent mixture of THF/MeOH/H2O (2/2/2 mL) was stirred at room temperature for 4 h, at which time it was brought to pH 5 by the addition of 2N HCl (aq). The mixture was extracted with EtOAc (3×). The combined extracts were dried over Na2SO4, filtered, and concentrated under reduced pressure. The resultant residue (crude compound 26d) was dried under reduced pressure for 18 h, and used in the following step without further purification.

후처리

  1. extractionThe mixture was extracted with EtOAc (3×)
  2. dry with materialThe combined extracts were dried over Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. dry with materialThe resultant residue (crude compound 26d) was dried under reduced pressure for 18 h
  6. customused in the following step without further purification

출처 및 근거

ORD 기록
ord-9bef944d31604288a8cd1d267d7e71c2
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08962607B2

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