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Hydrochloric Acid → 4-[(2R)-2-methylpiperidin-1-yl]-3-(trifluoromethyl)benzoic acid

HRID 400768
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인쇄 미리보기

반응식

HRID 400768 반응식
[CH3:1][C@@H:2]1[CH2:7][CH2:6][CH2:5][CH2:4][N:3]1[C:8]1[CH:15]=[CH:14][C:11]([C:12]#N)=[CH:10][C:9]=1[C:16]([F:19])([F:18])[F:17].[OH-:20].[Na+].Cl.C[OH:24]>O>[CH3:1][C@@H:2]1[CH2:7][CH2:6][CH2:5][CH2:4][N:3]1[C:8]1[CH:15]=[CH:14][C:11]([C:12]([OH:24])=[O:20])=[CH:10][C:9]=1[C:16]([F:19])([F:18])[F:17]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 14798Sodium HydroxideHCID 666775804-[(2R)-2-methylpiperidin-1-yl]-3-(trifluoromethyl)benzonitrile

생성물 1

HCID 580662284-[(2R)-2-methylpiperidin-1-yl]-3-(trifluoromethyl)benzoic acid

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
100 °C

실험 절차

4-[(2R)-2-methylpiperidin-1-yl]-3-(trifluoromethyl)benzonitrile (1.40 g; 5.22 mmol; 1 eq.) was dissolved in MeOH (7 mL) to which was added NaOH (5 N solution in water, 7 mL). The reaction mixture was heated to 100° C. for 7 hours. The reaction mixture was acidified to pH 2 with 5N HCl solution in water. The resulting precipitate was filtered and washed with water to give a light brown solid. It was recrystallized from Et2O/cHex to give a beige solid.

후처리

  1. filtrationThe resulting precipitate was filtered
  2. washwashed with water
  3. customto give a light brown solid
  4. customIt was recrystallized from Et2O/cHex
  5. customto give a beige solid

출처 및 근거

ORD 기록
ord-80be446b6e6e46c6ba33e3de85df24f4
출처 데이터셋
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08741923B2

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