반응식
C1CN([P+](ON2N=NC3C=CC=CC2=3)(N2CCCC2)N2CCCC2)CC1.F[P-](F)(F)(F)(F)F.[CH3:34][O:35][P:36]([CH:39]([NH:43][C:44]([O:46][CH2:47][C:48]1[CH:53]=[CH:52][CH:51]=[CH:50][CH:49]=1)=[O:45])[CH:40]([CH3:42])[CH3:41])(=O)[OH:37].[CH3:54][O:55][C:56](=[O:70])[CH:57]([OH:69])[CH2:58][CH2:59][CH2:60][NH:61][C:62]([O:64][C:65]([CH3:68])([CH3:67])[CH3:66])=[O:63].CCN(C(C)C)C(C)C>CN(C=O)C.C(OCC)(=O)C>[CH3:54][O:55][C:56](=[O:70])[CH:57]([O:69][P:36]([CH:39]([NH:43][C:44]([O:46][CH2:47][C:48]1[CH:53]=[CH:52][CH:51]=[CH:50][CH:49]=1)=[O:45])[CH:40]([CH3:42])[CH3:41])([O:35][CH3:34])=[O:37])[CH2:58][CH2:59][CH2:60][NH:61][C:62]([O:64][C:65]([CH3:67])([CH3:66])[CH3:68])=[O:63]참가 물질
7
반응물 4
생성물 1
시약·촉매·용매 2
실험 절차
A solution of PyBOP (2.1 g, 4.0 mmol) in DMF (3 mL) was added to a mixture of (1-benzyloxycarbonylamino-2-methyl-propyl)-phosphonic acid monomethyl ester (1.0 g, 3.32 mmol) and 5-tert-butoxycarbonylamino-2-hydroxy-pentanoic acid methyl ester (865 mg, 3.5 mmol) in DMF (4 mL) under argon. DIPEA (2.28 mL, 13.3 mmol) was added dropwise and the mixture was stirred over night. Ethyl acetate was added and the mixture was washed with 10% KHSO4, satd. NaHCO3 and brine and dried. Concentration under reduced pressure followed by chromathography (heptane/EtOAc, 1:1→1:6) gave 2-[(1-benzyloxycarbonylamino-2-methyl-propyl)-methoxy-phosphinoyloxy]-5-tert-butoxycarbonylamino-pentanoic acid methyl ester (1.21 g, 69%).
후처리
- washthe mixture was washed with 10% KHSO4
- dry with materialNaHCO3 and brine and dried
- concentrationConcentration under reduced pressure
출처 및 근거
- ORD 기록
- ord-b6f4d112812d4f00b22a247b00911401
- 출처 데이터셋
- uspto-grants-2008_09
- 특허 번호
- US07423012B2
연결된 노트
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