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1,2-Dichloroethane → HCID 22249396, 화합물

HRID 887528
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HRID 887528 반응식
[CH3:1][C:2]1([CH3:14])[C:10]2[C:5](=[CH:6][C:7]([N+:11]([O-:13])=[O:12])=[CH:8][CH:9]=2)[NH:4][CH2:3]1.C1[CH:20]=[N:19][C:18]2N(O)N=NC=2C=1.[CH2:25](Cl)[CH2:26]Cl.CN(C=[O:33])C>C(Cl)Cl>[CH3:18][N:19]([CH3:20])[CH2:25][C:26]([N:4]1[C:5]2[C:10](=[CH:9][CH:8]=[C:7]([N+:11]([O-:13])=[O:12])[CH:6]=2)[C:2]([CH3:14])([CH3:1])[CH2:3]1)=[O:33]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 111,2-DichloroethaneHCID 6228DimethylformamideHCID 181649HOAtHCID 219594663,3-Dimethyl-6-nitroindoline

생성물 1

HCID 22249396HCID 22249396, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

3,3-Dimethyl-6-nitro-2,3-dihydro-1H-indole (5 g) was dissolved in DMF (100 ml) and HOAt (3.89 g) dimethylamino-acetic acid (5.83 g) and EDC (3.89 g) were added. The reaction was stirred overnight. The mixture was diluted with CH2Cl2 (1 L) and washed with sat'd NaHCO3 (3×200 ml). The organic layer was washed with brine, dried over Na2SO4, filtered and concentrated in vacuo. The residue was purified by flash chromatography (SiO2, EtOAc to 5% MeOH/EtOAc) to afford the title compound.

후처리

  1. washwashed with sat'd NaHCO3 (3×200 ml)
  2. washThe organic layer was washed with brine
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified by flash chromatography (SiO2, EtOAc to 5% MeOH/EtOAc)

출처 및 근거

ORD 기록
ord-4cc5b36c4f1c44329e518ff7d251c062
출처 데이터셋
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08247430B2

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