反応式
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]参加物
7
反応物 4
生成物 1
試薬・触媒・溶媒 2
実験手順
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%).
後処理
- washthe mixture was washed with 10% KHSO4
- dry with materialNaHCO3 and brine and dried
- concentrationConcentration under reduced pressure
出典と根拠
- ORDレコード
- ord-b6f4d112812d4f00b22a247b00911401
- 出典データセット
- uspto-grants-2008_09
- 特許番号
- US07423012B2
関連ノート
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