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

HRID 1968600
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HRID 1968600 반응식
[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
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 21899815
MeOH tetrahydrofuran
용매

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온도
60 °C

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-f868e359823745e8bcd70127cd13138c
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08426422B2

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