Formamide → 4-hydroxy-N-methylproline

HRID 9940

반응식

HRID 9940 반응식
[CH2:1]1[C@@H:5]([C:6]([OH:8])=[O:7])[NH:4][CH2:3][C@@H:2]1[OH:9].[CH:10](N)=O.[H][H]>[Pd].O.C(O)C>[OH:9][C@H:2]1[CH2:3][N:4]([CH3:10])[C@H:5]([C:6]([OH:8])=[O:7])[CH2:1]1

참가 물질

7

반응물 3

HCID 713FormamideHCID 5810L-HydroxyprolineHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 117687004-hydroxy-N-methylproline수율 92.1%

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 702Ethanol용매HCID 962Water용매

실험 절차

A suspension of (2S,4R)-trans-4-hydroxyproline (5 g), 37% aqueous formamide solution (4.6 g) and 7.5% palladium on charcoal (53% water content, 3.2 g) in water (15 mL) was stirred at room temperature in an atmosphere of high-pressure hydrogen for 10 hours. After removing the palladium on charcoal by filtration, the water of the filtrate was removed by distillation under reduced pressure. The solid residue thus obtained was suspended and stirred in ethanol (25 mL). The crystals which precipitated were collected by filtration to give the title compound (5.1 g, yield 92%).

후처리

  1. customAfter removing the palladium on charcoal
  2. filtrationby filtration
  3. customthe water of the filtrate was removed by distillation under reduced pressure
  4. customThe solid residue thus obtained
  5. customThe crystals which precipitated
  6. filtrationwere collected by filtration

출처 및 근거

ORD 기록
ord-9c8bc77dc55d4a88890aa30b737c9dda
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07091363B2

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