Methanol → HCID 14102971、化合物

HRID 2275635ノート

反応式

HRID 2275635 の反応式
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

参加物

7

反応物 5

HCID 887MethanolHCID 6344DichloromethaneHCID 6422Trifluoroacetic acidHCID 86602285HCID 86602285、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 14102971HCID 14102971、化合物

試薬・触媒・溶媒 1

HCID 23938Palladium触媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-39e7e0229fda40cc823332a3afa7d77c
出典データセット
uspto-grants-2015_09
特許番号
US09126927B2

反応ノート

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