Methanol → HCID 14102971, 화합물

HRID 504385노트

반응식

HRID 504385 반응식
O[C:2]1([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH2:6][N:5](C(OC(C)(C)C)=O)[C@H:4]([C:14]([O:16][CH3:17])=[O:15])[CH2:3]1.FC(F)(F)C(O)=O.C(Cl)Cl.CO.[H][H]>[Pd]>[C:18]1([C@@H:2]2[CH2:6][NH:5][C@H:4]([C:14]([O:16][CH3:17])=[O:15])[CH2:3]2)[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1

참가 물질

7

반응물 5

HCID 887MethanolHCID 6344DichloromethaneHCID 6422Trifluoroacetic acidHCID 86602285HCID 86602285, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 14102971HCID 14102971, 화합물

시약·촉매·용매 1

HCID 23938Palladium촉매

실험 절차

1-tert-Butyl 2-methyl (2S)-4-hydroxy-4-phenylpyrrolidine-1,2-dicarboxylate (0.32 g, 0.0010 mol) was treated with trifluoroacetic acid (1.00 mL, 0.0130 mol) and methylene chloride (1.00 mL, 0.0156 mol) at rt for 4 h. The solvents were evaporated and the residue was dissolved in methanol (5.0 mL, 0.12 mol). Palladium (50.0 mg, 0.000470 mol) was added under nitrogen and the resulting mixture was hydrogenized with a hydrogen-gas-filled-balloon for 3 h. The mixture was filtered and the filtrate was concentrated to give the desired product, which was directly used in the next step without further purification.

후처리

  1. customThe solvents were evaporated
  2. additiongas-filled-balloon for 3 h
  3. filtrationThe mixture was filtered
  4. concentrationthe filtrate was concentrated

출처 및 근거

ORD 기록
ord-e1e2c03226aa498a96845228008bbcfc
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07776874B2

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