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

HRID 1177935

反応式

HRID 1177935 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 21881883Oxolane--water (1/1)溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-e3ae7b1d8a90423cacf494b73e07d6df
出典データセット
uspto-grants-2010_11
特許番号
US07842696B2

関連ノート

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