Trifluoroacetic acid → HCID 11056701, 화합물

HRID 1099202노트

반응식

HRID 1099202 반응식
[C:1]([N:4]1[CH:8](O)[CH2:7][CH:6]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[C:5]1([C:21]([O:23][CH2:24][CH3:25])=[O:22])[C:16]([O:18][CH2:19][CH3:20])=[O:17])(=[O:3])[CH3:2].C([SiH](CC)CC)C.FC(F)(F)C(O)=O>ClCCl>[C:1]([N:4]1[CH2:8][CH2:7][CH:6]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[C:5]1([C:21]([O:23][CH2:24][CH3:25])=[O:22])[C:16]([O:18][CH2:19][CH3:20])=[O:17])(=[O:3])[CH3:2]

참가 물질

5

반응물 3

HCID 6422Trifluoroacetic acidHCID 12052TriethylsilaneHCID 658963Diethyl 1-acetyl-5-hydroxy-3-phenylpyrrolidine-2,2-dicarboxylate

생성물 1

HCID 11056701HCID 11056701, 화합물수율 100%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of diethyl 1-acetyl-5-hydroxy-3-phenylpyrrolidine-2,2-dicarboxylate (116.0 g, 331 mmol) and triethylsilane (80 ml, 497 mmol) in dichloromethane (675 ml) was added trifluoroacetic acid (254 ml, 3.32 mol) dropwise with stirring over 45 min. The reaction was allowed to stir for 2.5 h at rt and was then concentrated and redissolved in EtOAc. The organics were washed with sat'd sodium bicarbonate, dried over sodium sulfate, filtered, and concentrated in vacuo to yield diethyl 1-acetyl-3-phenylpyrrolidine-2,2-dicarboxylate as an oil (100%).

후처리

  1. stirringto stir for 2.5 h at rt
  2. concentrationwas then concentrated
  3. dissolutionredissolved in EtOAc
  4. washThe organics were washed with sat'd sodium bicarbonate
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-7adb26d3ec474856b0550f6b9a4e5dd4
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08143405B2

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