Trifluoroacetic acid → HCID 178420112, 화합물

HRID 1443380노트

반응식

HRID 1443380 반응식
FC(F)(F)C(O)=O.C(OC([N:15]1[CH:24]([C:25]2[NH:26][CH:27]=[C:28]([C:30]3[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=3)[N:29]=2)[CH2:23][C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[CH2:16]1)=O)(C)(C)C>>[C:30]1([C:28]2[N:29]=[C:25]([CH:24]3[CH2:23][C:22]4[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=4)[CH2:16][NH:15]3)[NH:26][CH:27]=2)[CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=1

참가 물질

3

반응물 2

HCID 6422Trifluoroacetic acidHCID 178451477HCID 178451477, 화합물

생성물 1

HCID 178420112HCID 178420112, 화합물

실험 절차

Triflouroacetic acid (TFA) (4 mL) was cooled in a test tube to about 0° C. To the cool solvent was then added the product prepared in Step B (0.75 g, 2 mmol) above. The reaction mixture was allowed to warm to room temperature over about 45 minutes. Excess TFA was removed under a stream of N2 gas. The residue was partitioned between dichloromethane (15 mL) and saturated NaHCO3. The aqueous phase was then re-extracted with a second portion of dichloromethane and the organic phases combined, dried over MgSO4 and filtered, to yield the title compound in dichloromethane solution. The filtrate was used in the next step without further purification or isolation.

후처리

  1. customExcess TFA was removed under a stream of N2 gas
  2. customThe residue was partitioned between dichloromethane (15 mL) and saturated NaHCO3
  3. extractionThe aqueous phase was then re-extracted with a second portion of dichloromethane
  4. dry with materialdried over MgSO4
  5. filtrationfiltered

출처 및 근거

ORD 기록
ord-2961d1d5d5cb4ea79e22f188918c74ac
출처 데이터셋
uspto-grants-2010_02
특허 번호
US07659402B2

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