반응식
Cl.[CH2:2]([O:9][NH2:10])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[OH-].[K+].[C:13]([O:17][C:18]([NH:20][CH2:21][C:22](O)=[O:23])=[O:19])([CH3:16])([CH3:15])[CH3:14].C(N(CC)CC)C.C(=O)=O.C(O)C.ClC(OCC(C)C)=O>CO.O1CCCC1>[C:13]([O:17][C:18]([NH:20][CH2:21][C:22]([NH:10][O:9][CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1)=[O:23])=[O:19])([CH3:16])([CH3:15])[CH3:14]참가 물질
반응물 6
생성물 1
시약·촉매·용매 2
실험 절차
O-Benzylhydroxylamine hydrochloride (15.0 g, 93.8 mMol) was dissolved in methanol (150 ml) and added to a solution of potassium hydroxide (5.27 g, 93.8 mMol) in methanol (50 ml). The resulting mixture was cooled, filtered, evaporated, dissolved in tetrahydrofuran (25 ml) and filtered as solution A. t-Butyloxycarbonyl glycine (16.4 g, 93.8 mMol) was dissolved in tetrahydrofuran (75 ml), triethylamine (13.2 ml, 93.8 mMol) added and the solution cooled to -10° C. with dry ice/ethanol. Iso-butyl chloroformate (12.2 ml, 93.8 mMol) was added and the solution stirred cold 2 minutes, before adding solution A dropwise. The mixture was stirred cold 1 hour and at room temperature 2 hours, filtered, evaporated, dissolved in ethyl acetate (100 ml), washed with water (3× 50 ml), dried over magnesium sulfate and evaporated to an oil.
후처리
- temperatureThe resulting mixture was cooled
- filtrationfiltered
- customevaporated
- dissolutiondissolved in tetrahydrofuran (25 ml)
- filtrationfiltered as solution A
- stirringThe mixture was stirred cold 1 hour and at room temperature 2 hours
- filtrationfiltered
- customevaporated
- dissolutiondissolved in ethyl acetate (100 ml)
- washwashed with water (3× 50 ml)
- dry with materialdried over magnesium sulfate
- customevaporated to an oil
출처 및 근거
- ORD 기록
- ord-564b064ae6d147c3b71798fedd0fe5c9
- 출처 데이터셋
- uspto-grants-1977_06
- 특허 번호
- US04028401
연결된 노트
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