Potassium Phosphate, Dibasic → 3-(S)-hydroxymethyl-4-(R)-tert.-butylsulphonyl-2-azetidinone

HRID 65439

반응식

HRID 65439 반응식
COC1C=CC(C[N:8]2[C@H:11]([S:12]([C:15]([CH3:18])([CH3:17])[CH3:16])(=[O:14])=[O:13])[C@@H:10]([CH2:19][OH:20])[C:9]2=[O:21])=CC=1.S(OOS([O-])(=O)=O)([O-])(=O)=O.[Na+].[Na+].P([O-])([O-])(O)=O.[K+].[K+]>C(#N)C.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Fe+2].O.C([O-])(=O)C.[Cu+2].C([O-])(=O)C>[OH:20][CH2:19][C@@H:10]1[C@@H:11]([S:12]([C:15]([CH3:17])([CH3:16])[CH3:18])(=[O:14])=[O:13])[NH:8][C:9]1=[O:21]

참가 물질

8

반응물 3

HCID 24450Potassium Phosphate, DibasicHCID 62655Sodium PersulfateHCID 186047721-p-methoxybenzyl-3-(S)-hydroxymethyl-4-(R)-tert.-butylsulphonyl-2-azetidinone

생성물 1

HCID 186047743-(S)-hydroxymethyl-4-(R)-tert.-butylsulphonyl-2-azetidinone

시약·촉매·용매 4

HCID 62662Ferrous sulfate heptahydrate촉매HCID 165397Cupric acetate monohydrate촉매HCID 962Water용매HCID 6342Acetonitrile용매

실험 절차

A solution of 68.3 mg (0.2 mmol) of 1-p-methoxybenzyl-3-(S)-hydroxymethyl-4-(R)-tert.-butylsulphonyl-2-azetidinone in 4 ml of acetonitrile is added to a solution of 428 mg (1.8 mmol) of sodium peroxydisulphate, 174 mg (1 mmol) of dipotassium hydrogen phosphate, 1 mg of iron(II) sulphate heptahydrate and 2 mg of copper(II) acetate hydrate in 4 ml of water. The mixture is stirred for 2 hours under an argon atmosphere at a bath temperature of 65°. The resulting mixture is then concentrated to half its volume under reduced pressure and extracted with ethyl acetate. The extract is triturated with methylene chloride and ether and the pure title compound is obtained.

후처리

  1. concentrationThe resulting mixture is then concentrated to half its volume under reduced pressure
  2. extractionextracted with ethyl acetate
  3. customThe extract is triturated with methylene chloride and ether

출처 및 근거

ORD 기록
ord-139ed6457cd64e2e9fcb010d4805aeea
출처 데이터셋
uspto-grants-1986_09
특허 번호
US04614614

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