Hydrochloric Acid → 4-(4-Methylpiperazin-1-yl)benzoic acid

HRID 1177935

반응식

HRID 1177935 반응식
[Li+].[OH-].C[O:4][C:5](=[O:19])[C:6]1[CH:11]=[CH:10][C:9]([N:12]2[CH2:17][CH2:16][N:15]([CH3:18])[CH2:14][CH2:13]2)=[CH:8][CH:7]=1.O.Cl>C1COCC1.O>[CH3:18][N:15]1[CH2:14][CH2:13][N:12]([C:9]2[CH:10]=[CH:11][C:6]([C:5]([OH:19])=[O:4])=[CH:7][CH:8]=2)[CH2:17][CH2:16]1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 3939Lithium HydroxideHCID 1472668Methyl 4-(4-methylpiperazin-1-yl)benzoate

생성물 1

HCID 7365324-(4-Methylpiperazin-1-yl)benzoic acid수율 85.13%

시약·촉매·용매 1

HCID 21881883Oxolane--water (1/1)용매

실험 절차

LiOH (67 mg, 1.6 mmol) was added to a stirred solution 4-(4-methyl-piperazin-1-yl)-benzoic acid methyl ester (124 mg, 0.73 mmol) in THF:H2O (1:1, 4 mL), and the resulting mixture was stirred at room temperature overnight. The reaction mixture was concentrated under reduced pressure to get the residue. Cold water was then added and acidified it with 10% aqueous HCl and concentrated under reduced pressure to afford 116 mg (85.13% yield) of 4-(4-methyl-piperazin-1-yl)-benzoic acid. 1H NMR (DMSO-D2O): δ 7.8 (d, 2H), 7.0 (d, 2H), 3.4 (s, 4H), 2.8 (s, 4H), 2.4 (s, 3H).

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customto get the residue
  3. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-e3ae7b1d8a90423cacf494b73e07d6df
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07842696B2

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