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Hydrochloric Acid → 4-[4-(3,3-Diphenylprop-2-en-1-yl)piperazin-1-yl]benzoic acid

HRID 1968600
ノート
印刷プレビュー

反応式

HRID 1968600 の反応式
[C:1]1([C:7]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)=[CH:8][CH2:9][N:10]2[CH2:15][CH2:14][N:13]([C:16]3[CH:26]=[CH:25][C:19]([C:20]([O:22]CC)=[O:21])=[CH:18][CH:17]=3)[CH2:12][CH2:11]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.O.[OH-].[Li+].Cl>O1CCCC1.CO.O>[C:27]1([C:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)=[CH:8][CH2:9][N:10]2[CH2:11][CH2:12][N:13]([C:16]3[CH:17]=[CH:18][C:19]([C:20]([OH:22])=[O:21])=[CH:25][CH:26]=3)[CH2:14][CH2:15]2)[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 168937Lithium hydroxide, monohydrateHCID 67144443Ethyl 4-(4-(3,3-diphenylallyl)piperazin-1-yl)benzoate

生成物 1

HCID 671447144-[4-(3,3-Diphenylprop-2-en-1-yl)piperazin-1-yl]benzoic acid

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 21899815
MeOH tetrahydrofuran
溶媒

反応条件

温度
60 °C

実験手順

To a solution of EXAMPLE 1C (10.00 g, 23.4 mmol) in tetrahydrofuran/methanol (100/50 mL) was added solution of lithium hydroxide monohydrate (2.59 g, 70 mmol) in water (30 mL). The reaction mixture was stirred at 60° C. for 16 hours, then was cooled to room temperature and the organic solvents were concentrated. The white solid residue was dissolved in hot water and then the product was neutralized with HCl (3 equivalents). After cooling to room temperature, the precipitate was filtered off, washed with water and dried in a vacuum oven overnight at 40° C.

後処理

  1. temperaturewas cooled to room temperature
  2. concentrationthe organic solvents were concentrated
  3. dissolutionThe white solid residue was dissolved in hot water
  4. temperatureAfter cooling to room temperature
  5. filtrationthe precipitate was filtered off
  6. washwashed with water
  7. customdried in a vacuum oven overnight at 40° C.

出典と根拠

ORDレコード
ord-f868e359823745e8bcd70127cd13138c
出典データセット
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08426422B2

反応ノート

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