Trifluoroacetic acid → HCID 91665637, 화합물

HRID 1035321노트

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HRID 1035321 반응식
[CH2:1]([N:8]([CH2:25][C:26]([O:28]CC)=O)[C:9](=[O:24])[C@H:10]([NH:16]C(OC(C)(C)C)=O)[CH2:11][C:12]([O:14][CH3:15])=[O:13])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.F[C:32](F)(F)C(O)=O>ClCCl>[CH2:1]([N:8]1[CH2:25][C:26](=[O:28])[NH:16][C@H:10]([CH2:11][C:12]([O:14][CH2:15][CH3:32])=[O:13])[C:9]1=[O:24])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 67248809HCID 67248809, 화합물

생성물 1

HCID 91665637HCID 91665637, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
70 °C

실험 절차

To a solution of Example 255C (50.75 g, 120 mmol) in dichloromethane (50 mL) was added trifluoroacetic acid. The reaction was stirred overnight and then concentrated. Ammonia was added (7 N, methanol, 250 mL) and the solution was warmed to 70° C. for 2 hours. The reaction was concentrated and dichloromethane was added (500 mL). The solution stirred for 10 minutes before the salt was removed by filtration. The solution was then concentrated and purification via flash chromatography (3% 2 N NH3 in methanol/dichloromethane) afforded the title compound.

후처리

  1. concentrationconcentrated
  2. additionAmmonia was added (7 N, methanol, 250 mL)
  3. concentrationThe reaction was concentrated
  4. additiondichloromethane was added (500 mL)
  5. stirringThe solution stirred for 10 minutes before the salt
  6. customwas removed by filtration
  7. concentrationThe solution was then concentrated
  8. custompurification via flash chromatography (3% 2 N NH3 in methanol/dichloromethane)

출처 및 근거

ORD 기록
ord-eaff4d23406047628cb7089bb2a458f0
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08546377B2

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