Trifluoroacetic acid → HCID 89852058, 화합물

HRID 627146노트

반응식

HRID 627146 반응식
[CH2:1]([O:4][N:5]([C@H:18]1[CH2:23][N:22](C(OC(C)(C)C)=O)[C@H:21]([CH2:31][O:32][CH3:33])[CH:20]=[C:19]1[C:34](=[O:36])[NH2:35])[S:6]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[N+:15]([O-:17])=[O:16])(=[O:8])=[O:7])[CH:2]=[CH2:3].FC(F)(F)C(O)=O>ClCCl>[CH2:1]([O:4][N:5]([C@@H:18]1[C:19]([C:34]([NH2:35])=[O:36])=[CH:20][C@@H:21]([CH2:31][O:32][CH3:33])[NH:22][CH2:23]1)[S:6]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[N+:15]([O-:17])=[O:16])(=[O:8])=[O:7])[CH:2]=[CH2:3]

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 89863149(2S,5R)-tert-butyl 5-(N-(allyloxy)-2-nitrophenylsulfonamido)-4-carbamoyl-2-(methoxymethyl)-5,6-dihydropyridine-1(2H)-carboxylate

생성물 1

HCID 89852058HCID 89852058, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of Intermediate 112 (729 mg, 1.38 mmol) in dichloromethane (10 mL) was added trifluoroacetic acid (2133 μl, 27.69 mmol). This solution was slightly darker after addition. The reaction was placed under a nitrogen atmosphere and stirred until LCMS analysis indicated consumption of starting material (˜45 minutes). At that time, solvent was removed in vacuo. The residue was taken up in toluene and sonicated, and then toluene was removed in vacuo. This was repeated twice, affording an orange solid of high purity by proton NMR. The product was taken forward without further purification.

후처리

  1. additionafter addition
  2. customconsumption of starting material (˜45 minutes)
  3. customAt that time, solvent was removed in vacuo
  4. customsonicated
  5. customtoluene was removed in vacuo
  6. customaffording an orange solid of high purity by proton NMR
  7. customThe product was taken forward without further purification

출처 및 근거

ORD 기록
ord-c91c1c4dcef440028f7e7a76c3efcb6c
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09309245B2

반응 노트

불러오는 중…