Lithium Hydroxide → 4-[4-(4-Trifluoromethyl-phenyl)-piperazin-1-yl]-butyric acid lithium salt

HRID 511066노트

반응식

HRID 511066 반응식
C([O:3][C:4](=[O:24])[CH2:5][CH2:6][CH2:7][N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:19]=[CH:18][C:17]([C:20]([F:23])([F:22])[F:21])=[CH:16][CH:15]=2)[CH2:10][CH2:9]1)C.[OH-].[Li+:26]>O1CCCC1.O.C(#N)C>[Li+:26].[F:23][C:20]([F:21])([F:22])[C:17]1[CH:18]=[CH:19][C:14]([N:11]2[CH2:12][CH2:13][N:8]([CH2:7][CH2:6][CH2:5][C:4]([O-:24])=[O:3])[CH2:9][CH2:10]2)=[CH:15][CH:16]=1

참가 물질

6

반응물 2

HCID 3939Lithium HydroxideHCID 585765934-[4-(4-Trifluoromethyl-phenyl)-piperazin-1-yl]-butyric acid ethyl ester

생성물 1

HCID 585760704-[4-(4-Trifluoromethyl-phenyl)-piperazin-1-yl]-butyric acid lithium salt

시약·촉매·용매 3

HCID 962Water용매HCID 6342Acetonitrile용매HCID 8028Tetrahydrofuran용매

실험 절차

4-[4-(4-Trifluoromethyl-phenyl)-piperazin-1-yl]-butyric acid ethyl ester (660 mg; 1.92 mmol, prepared in accordance with Example 2) and lithium hydroxide are dissolved in a mixture of tetrahydrofuran (2.8 mL) and water (1.2 mL). The resulting mixture is irradiated in a mono-mode microwave oven for 30 minutes at 70° C. The mixture is then diluted with acetonitrile (20 mL) and the precipitate formed is filtered and rinsed with acetonitrile (10 mL). The solid obtained is then dried under high vacuum to deliver the desired product (584 mg; 1.81 mmol).

후처리

  1. customThe resulting mixture is irradiated in a mono-mode microwave oven for 30 minutes at 70° C
  2. customthe precipitate formed
  3. filtrationis filtered
  4. washrinsed with acetonitrile (10 mL)
  5. customThe solid obtained
  6. customis then dried under high vacuum

출처 및 근거

ORD 기록
ord-ce965d0904984e019d4eeca57770a8e7
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09096524B2

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