1,2-Dichloroethane → HCID 58713650、化合物

HRID 475505ノート

反応式

HRID 475505 の反応式
[CH2:1]([N:8]1[C:12]2[CH2:13][C:14](=[O:16])[CH2:15][C:11]=2[C:10]([C:17]([OH:19])=[O:18])=[N:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O[N:21]1[C:25](=[O:26])[CH2:24][CH2:23][C:22]1=[O:27].C(Cl)CCl>C(Cl)Cl>[O:27]=[C:22]1[CH2:23][CH2:24][C:25](=[O:26])[N:21]1[O:18][C:17]([C:10]1[C:11]2[CH2:15][C:14](=[O:16])[CH2:13][C:12]=2[N:8]([CH2:1][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)[N:9]=1)=[O:19]

参加物

5

反応物 3

HCID 111,2-DichloroethaneHCID 80170N-HydroxysuccinimideHCID 23135167HCID 23135167、化合物

生成物 1

HCID 58713650HCID 58713650、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of the intermediate from step C (1.34 g, 5.25 mmol) in CH2Cl2 (50 mL) was added N-hydroxy succinimide (1.21 g, 10.5 mmol) followed by EDC (2.01 g, 10.5 mmol). After stirring at room temperature for 18 hours, the reaction mixture was concentrated in vacuo. The residue was diluted with ethyl acetate (200 mL), washed with saturated NaHCO3, solution and brine. The organic layer was dried over anhydrous Na2SO4, filtered and concentrated in vacuo. A yellow solid was obtained.

後処理

  1. concentrationthe reaction mixture was concentrated in vacuo
  2. additionThe residue was diluted with ethyl acetate (200 mL)
  3. washwashed with saturated NaHCO3, solution and brine
  4. dry with materialThe organic layer was dried over anhydrous Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customA yellow solid was obtained

出典と根拠

ORDレコード
ord-10c5674a07b24b0c8b285edd34f5121b
出典データセット
uspto-grants-2014_01
特許番号
US08637555B2

反応ノート

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