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Ammonia → (rac)-2-(4-(4-(Trifluoromethyl)phenyl)-6,7-dihydro-5H-cyclopenta[c]pyridin-7-yloxy)acetamide

HRID 714110
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인쇄 미리보기

반응식

HRID 714110 반응식
Cl.[F:2][C:3]([F:25])([F:24])[C:4]1[CH:9]=[CH:8][C:7]([C:10]2[C:11]3[CH2:18][CH2:17][CH:16]([O:19][CH2:20][C:21]([OH:23])=O)[C:12]=3[CH:13]=[N:14][CH:15]=2)=[CH:6][CH:5]=1.C(N1C=CN=C1)([N:28]1C=CN=C1)=O.N>CN(C=O)C.C(Cl)Cl>[F:24][C:3]([F:2])([F:25])[C:4]1[CH:5]=[CH:6][C:7]([C:10]2[C:11]3[CH2:18][CH2:17][CH:16]([O:19][CH2:20][C:21]([NH2:28])=[O:23])[C:12]=3[CH:13]=[N:14][CH:15]=2)=[CH:8][CH:9]=1
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참가 물질

6

반응물 3

HCID 222Ammonia2회HCID 682631,1'-Carbonyldiimidazole2회HCID 89846289(rac)-2-(4-(4-(Trifluoromethyl)phenyl)-6,7-dihydro-5H-cyclopenta[c]pyridin-7-yloxy)acetic acid hydrochloride

생성물 1

HCID 71811452(rac)-2-(4-(4-(Trifluoromethyl)phenyl)-6,7-dihydro-5H-cyclopenta[c]pyridin-7-yloxy)acetamide수율 48%

시약·촉매·용매 2

HCID 6228
Dimethylformamide
용매
HCID 6344Dichloromethane용매

실험 절차

To a solution of (rac)-2-(4-(4-(trifluoromethyl)phenyl)-6,7-dihydro-5H-cyclopenta[c]pyridin-7-yloxy)acetic acid hydrochloride (example 99) (34.6 mg, 0.093 mmol) in DMF (1 mL) was added N,N-triethylamine (31 μL, 0.22 mmol) and 1,1′-carbonyldiimidazole (18.0 mg, 0.11 mmol). The reaction was stirred at room temperature for 2 h, cooled (0°) and treated with aq. 25% ammonia solution (0.87 mL, 5.55 mmol) and evaporated after 30 min to give a 1:1 mixture of starting material and product. The residue was dissolved in CH2Cl2, dried (Na2SO4) and evaporated. The oil was again dissolved in DMF (1 mL) and N,N-triethylamine (15.5 μL, 0.11 mmol) and 1,1′-carbonyldiimidazole (18.0 mg, 0.11 mmol) were added. The reaction was stirred at room temperature for 2 h, cooled (0°) and treated with aq. 25% ammonia solution (0.87 mL, 5.55 mmol) and evaporated after 30 min at room temperature. The solution was evaporated, dried in vacuo and purified by flash chromatography (20 g SiO2, Telos-cartridge, 3% MeOH in CH2Cl2) to give the title compound (15 mg, 48%) as off-white solid. MS: 337.1 (M+H+).

후처리

  1. temperaturecooled (0°)
  2. customevaporated after 30 min
  3. customto give
  4. additiona 1:1 mixture of starting material and product
  5. dry with materialdried (Na2SO4)
  6. customevaporated
  7. dissolutionThe oil was again dissolved in DMF (1 mL)
  8. stirringThe reaction was stirred at room temperature for 2 h
  9. temperaturecooled (0°)
  10. customevaporated after 30 min at room temperature
  11. customThe solution was evaporated
  12. customdried in vacuo
  13. custompurified by flash chromatography (20 g SiO2, Telos-cartridge, 3% MeOH in CH2Cl2)

출처 및 근거

ORD 기록
ord-bf5a543fd143474d8716047ae224bb3f
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09187429B2

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