HCID 54281127, 화합물 → 3-hydroxyaniracetam

HRID 1462942노트

반응식

HRID 1462942 반응식
[CH3:1][O:2][C:3]1[CH:18]=[CH:17][C:6]([C:7]([NH:9][CH2:10][CH2:11][C@@H:12]([OH:16])[C:13](O)=[O:14])=[O:8])=[CH:5][CH:4]=1>FC(F)(F)C(OC(=O)C(F)(F)F)=O.FC(F)(F)C([O-])=O.[Na+]>[CH3:1][O:2][C:3]1[CH:18]=[CH:17][C:6]([C:7]([N:9]2[CH2:10][CH2:11][C@@H:12]([OH:16])[C:13]2=[O:14])=[O:8])=[CH:5][CH:4]=1

참가 물질

4

반응물 1

HCID 54281127HCID 54281127, 화합물

생성물 1

HCID 1741273-hydroxyaniracetam

시약·촉매·용매 2

HCID 9845Trifluoroacetic anhydride용매HCID 517019Sodium Trifluoroacetate용매

실험 절차

1.05 g of (R)-4-(p-methoxybenzoylamino)-2-hydroxy-butyric acid are boiled at reflux for 48 hours while stirring in 8.5 ml of trifluoroacetic acid anhydride and 0.2 g of sodium trifluoroacetate. After evaporation of the mixture, the residue is shaken twice with toluene and the toluene is then removed by evaporation in vacuo. The residue, containing (R)-1-(p-methoxybenzoyl)-2-oxo-3-pyrrolidinyl-trifluoroacetate, is boiled at reflux for 30 minutes in absolute methanol. After evaporation of the methanol, the residue is boiled in 400 ml of diisopropyl ether, the mixture is decanted, the solution is concentrated to 140 ml and then stirred at room temperature. The solid is filtered off and there is obtained (R)-1-(p-methoxybenzoyl)-3-hydroxy-2-pyrrolidinone of melting point 122.5°-123° C.; [α]D20 =+207°; [α]54620 =+256°; [α]36520 =+1172° (c=1.0 in chloroform).

후처리

  1. temperatureat reflux for 48 hours
  2. customAfter evaporation of the mixture
  3. customthe toluene is then removed by evaporation in vacuo
  4. additionThe residue, containing (R)-1-(p-methoxybenzoyl)-2-oxo-3-pyrrolidinyl-trifluoroacetate
  5. temperatureat reflux for 30 minutes in absolute methanol
  6. customAfter evaporation of the methanol
  7. customthe mixture is decanted
  8. concentrationthe solution is concentrated to 140 ml
  9. stirringstirred at room temperature
  10. filtrationThe solid is filtered off

출처 및 근거

ORD 기록
ord-6c78d9a1abfe48139d97fcdd647aa721
출처 데이터셋
uspto-grants-1984_07
특허 번호
US04461906

반응 노트

불러오는 중…