Trifluoroacetic acid → HCID 57265194, 화합물

HRID 2396376노트

반응식

HRID 2396376 반응식
[C:1]1([S:7]([CH2:10][NH:11][C:12]2[C:20]3[C:15](=[CH:16][C:17]([Cl:29])=[C:18](C(OC(C)(C)C)=O)[C:19]=3[Cl:21])[NH:14][C:13]=2[C:30]([O:32][CH2:33][CH3:34])=[O:31])(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.FC(F)(F)C(O)=O>C(Cl)Cl>[C:1]1([S:7]([CH2:10][NH:11][C:12]2[C:20]3[C:15](=[CH:16][C:17]([Cl:29])=[CH:18][C:19]=3[Cl:21])[NH:14][C:13]=2[C:30]([O:32][CH2:33][CH3:34])=[O:31])(=[O:8])=[O:9])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 67705862HCID 67705862, 화합물

생성물 1

HCID 57265194HCID 57265194, 화합물수율 22%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Dissolve 3-[(phenylsulfonyl)methylamino]-2-carbethoxy-4,6-dichloro-tert-butyloxycarbonyl-indole (400 mg, 0.758 mmol) in methylene chloride (15 mL). Add, by dropwise addition, trifluoroacetic acid (15 mL) and stir at room temperature for 3 hours. Evaporate the solvent in vacuo and treat the resulting residue with saturated sodium hydrogen carbonate. Extract into methylene chloride and dry (MgSO4). Recrystallize (ethyl acetate/hexane) to give the title compound (70 mg, 22%); mp 244°-45° C.

후처리

  1. customEvaporate the solvent in vacuo
  2. additiontreat the resulting residue with saturated sodium hydrogen carbonate
  3. extractionExtract into methylene chloride
  4. dry with materialdry (MgSO4)
  5. customRecrystallize (ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-778386e51e2547f9b0446694f2f5cae8
출처 데이터셋
uspto-grants-1996_02
특허 번호
US05491153

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