1,2-Dichloroethane → HCID 51354039、化合物

HRID 2367552ノート

反応式

HRID 2367552 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].[NH2:19][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: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 6115AnilineHCID 181649HOAtHCID 51356009HCID 51356009、化合物

生成物 1

HCID 51354039HCID 51354039、化合物収率 76.6%

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 aniline (0.088 mL, 0.964 mmol), HOAt (0.131 g, 0.964 mmol) and EDC (0.222 g, 1.157 mmol), and the reaction mixture was stirred at room temperature overnight. The reaction mixture was washed with water (2×), and the organics were dried over Na2SO4 and concentrated to afford the title compound (0.247 g) as a brown oil. LC-MS (ES) m/z=240 [M+H]+.

後処理

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

出典と根拠

ORDレコード
ord-53738a7a311f4cc29a4f1c12d9588519
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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