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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Trifluoroacetic acid → HCID 57520094, 화합물

HRID 1528099
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HRID 1528099 반응식
[F:1][C:2]([F:37])([F:36])[C:3]1[N:8]=[C:7]([NH:9][C:10](=[O:35])[NH:11][C:12]2[C:21]3[C:16](=[CH:17][CH:18]=[C:19]([C:22]4[CH2:23][CH2:24][N:25](C(OC(C)(C)C)=O)[CH2:26][CH:27]=4)[CH:20]=3)[N:15]=[CH:14][CH:13]=2)[CH:6]=[CH:5][CH:4]=1.C(O)(C(F)(F)F)=O>C(Cl)Cl>[NH:25]1[CH2:26][CH:27]=[C:22]([C:19]2[CH:20]=[C:21]3[C:16](=[CH:17][CH:18]=2)[N:15]=[CH:14][CH:13]=[C:12]3[NH:11][C:10]([NH:9][C:7]2[CH:6]=[CH:5][CH:4]=[C:3]([C:2]([F:36])([F:37])[F:1])[N:8]=2)=[O:35])[CH2:23][CH2:24]1
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참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 57520093HCID 57520093, 화합물

생성물 1

HCID 57520094HCID 57520094, 화합물수율 80.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

0.2 g of tert-butyl 4-{4-[3-(6-trifluoromethyl-pyridin-2-yl)-ureido]-quinolin-6-yl}-3,6-dihydro-2H-pyridine-1-carboxylate (0.389 mmol) were dissolved in 0.6 ml DCM (yellow solution). 0.300 ml of TFA (3.89 mmol) were added and the reaction mixture was stirred for 2 h at RT. After evaporation of the solvent and excess TFA in vacuum, water was added to the residue, the acidic mixture extracted with ethyl acetate, the water phase adjusted to pH 9 with 1M NaOH and subsequently extracted three times with DCM. The combined DCM solutions were washed with a small amount of brine, dried over sodium sulphate and the solvent was removed in vacuum. 130 mg of the desired product were obtained as light yellow powder (yield: 81%).

후처리

  1. customAfter evaporation of the solvent and excess TFA in vacuum, water
  2. additionwas added to the residue
  3. extractionthe acidic mixture extracted with ethyl acetate
  4. extractionsubsequently extracted three times with DCM
  5. washThe combined DCM solutions were washed with a small amount of brine
  6. dry with materialdried over sodium sulphate
  7. customthe solvent was removed in vacuum

출처 및 근거

ORD 기록
ord-e1b7751bd9c0472e9f8a8e0862e1abc4
출처 데이터셋
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09090592B2

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