反応式
[CH2:1]([O:8][C:9]([NH:11][C@H:12]1[CH2:16][CH2:15][N:14]([C@@H:17]([CH3:21])[C:18]([OH:20])=O)[C:13]1=[O:22])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.F[B-](F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2C=CC=CC=2N=N1.C(N(CC)C(C)C)(C)C.[NH:54]1[CH2:59][CH2:58][O:57][CH2:56][CH2:55]1.[Cl-].[NH4+]>CN(C=O)C>[CH3:21][C@H:17]([N:14]1[CH2:15][CH2:16][C@H:12]([NH:11][C:9](=[O:10])[O:8][CH2:1][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)[C:13]1=[O:22])[C:18]([N:54]1[CH2:59][CH2:58][O:57][CH2:56][CH2:55]1)=[O:20]参加物
7
反応物 5
生成物 1
試薬・触媒・溶媒 1
実験手順
(2S)-2-((3S)-3-{[(Benzyloxy)carbonyl]amino}-2-oxopyrrolidin-1-yl)propanoic acid (84.5 g) was dissolved in DMF (2I) and O-(benzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium tetrafluoroborate (161 g) was added, followed by N,N-diisopropylethylamine (92 ml) and morpholine (46 ml). The mixture was stirred under nitrogen for 2.5 h, and saturated aqueous ammonium chloride was added. The mixture was stirred for 15 min then partitioned between water and ethyl acetate. The separated organic phase was washed with lithium chloride (10% by weight), followed by saturated sodium bicarbonate and brine. The organic layer was dried (over sodium sulphate) and concentrated under reduced pressure to give the title compound (65 g) as a yellow solid.
後処理
- stirringThe mixture was stirred for 15 min
- customthen partitioned between water and ethyl acetate
- washThe separated organic phase was washed with lithium chloride (10% by weight)
- dry with materialThe organic layer was dried (over sodium sulphate)
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-da9cd41501664b12815cadc2aacf7368
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07084139B2
関連ノート
読み込み中…