1,2-Dichloroethane → HCID 58713650, 화합물

HRID 475505노트

반응식

HRID 475505 반응식
[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]

참가 물질

5

반응물 3

HCID 111,2-DichloroethaneHCID 80170N-HydroxysuccinimideHCID 23135167HCID 23135167, 화합물

생성물 1

HCID 58713650HCID 58713650, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-10c5674a07b24b0c8b285edd34f5121b
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08637555B2

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