1,2-Dichloroethane → HCID 58504456、化合物

HRID 2367560ノート

反応式

HRID 2367560 の反応式
[CH3:1][C:2]([O:5][C:6]([N:8]1[C@H:13]([CH2:14][CH3:15])[CH2:12][O:11][C@H:10]([C:16]([OH:18])=O)[CH2:9]1)=[O:7])([CH3:4])[CH3:3].[CH2:19]([NH2:26])[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1.C1C=NC2N(O)N=NC=2C=1.C(Cl)CCl>C(Cl)Cl>[CH2:14]([C@H:13]1[N:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:9][C@@H:10]([C:16]([NH:26][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[O:18])[O:11][CH2:12]1)[CH3:15]

参加物

6

反応物 4

HCID 111,2-DichloroethaneHCID 7504BenzylamineHCID 181649HOAtHCID 51356009HCID 51356009、化合物

生成物 1

HCID 58504456HCID 58504456、化合物収率 105.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To (2S,5R)-4-{[(1,1-dimethylethyl)oxy]carbonyl}-5-ethyl-2-morpholinecarboxylic acid (0.390 g, 1.504 mmol) in CH2Cl2 (10 mL) were added benzylamine (0.164 mL, 1.504 mmol), HOAt (0.205 g, 1.504 mmol) and EDC (0.346 g, 1.805 mmol). The reaction was stirred at room temperature overnight. The reaction mixture was washed with H2O (3×) and the organics were then dried over Na2SO4 and concentrated to afford the title compound (0.551 g). LC-MS (ES) m/z=249 [M+H-Boc]+.

後処理

  1. washThe reaction mixture was washed with H2O (3×)
  2. dry with materialthe organics were then dried over Na2SO4
  3. concentrationconcentrated

出典と根拠

ORDレコード
ord-2ebf1f1c9bde4752a8961ca534832551
出典データセット
uspto-grants-2014_04
特許番号
US08697685B2

反応ノート

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