1,2-Dichloroethane → HCID 58504507、化合物

HRID 2367555ノート

反応式

HRID 2367555 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].[CH:19]1([NH2:25])[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]1.C1C=NC2N(O)N=NC=2C=1.C(Cl)CCl>C(Cl)Cl>[CH:19]1([NH:25][C:16]([C@H:10]2[O:11][CH2:12][C@@H:13]([CH2:14][CH3:15])[N:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:9]2)=[O:18])[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]1

参加物

6

反応物 4

HCID 111,2-DichloroethaneHCID 7965CyclohexylamineHCID 181649HOAtHCID 51356009HCID 51356009、化合物

生成物 1

HCID 58504507HCID 58504507、化合物収率 90.2%

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 (0.250 g, 0.964 mmol) in CH2Cl2 (10 mL) were added cyclohexylamine (0.096 g, 0.964 mmol), HOAt (0.131 g, 0.964 mmol) and EDC (0.222 g, 1.157 mmol), and the reaction was stirred at room temperature overnight. The reaction mixture was washed with H2O (2×) and the organics were dried over Na2SO4 and concentrated to afford the title compound (0.296 g) as a brown oil. LC-MS (ES) m/z=241 [M+H-Boc]+.

後処理

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

出典と根拠

ORDレコード
ord-5ccd88d43369409ab3f8a069081adb18
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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