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Benzamide, 2-chloro-6-nitro- → HCID 91152696, 화합물

HRID 1292949
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HRID 1292949 반응식
[Cl:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([N+:11]([O-])=O)[C:3]=1[C:4]([NH2:6])=[O:5].O=[CH:15][CH2:16][NH:17][C:18](=[O:24])[O:19][C:20]([CH3:23])([CH3:22])[CH3:21]>C(O)(=O)C.[Fe]>[Cl:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]2[C:3]=1[C:4](=[O:5])[NH:6][CH:15]([CH2:16][NH:17][C:18](=[O:24])[O:19][C:20]([CH3:23])([CH3:22])[CH3:21])[NH:11]2
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참가 물질

5

반응물 2

HCID 86279Benzamide, 2-chloro-6-nitro-HCID 4247255tert-butyl N-(2-oxoethyl)carbamate

생성물 1

HCID 91152696HCID 91152696, 화합물수율 21.4%

시약·촉매·용매 2

HCID 23925Iron촉매HCID 176Acetic Acid용매

실험 절차

A mixtre of 2-chloro-6-nitrobenzamide (0.3 g), iron powder (0.5 g) and t-butyl (N-2-oxoethyl)carbamate (1.0 g) in glacial acetic acid (5 mL) was heated at 50-55° C. for 2 h. The mixture was concentrated and the residue was partitioned between sat. NaHCO3 and EtOAc. The organic layer was dried (MgSO4), concentrated, and the residue was subjected to flash chromatography (silica gel/heptane-EtOAc 100:0 to 20:80 gradient) to afford the title compound as an off-white solid (0.1 g).

후처리

  1. concentrationThe mixture was concentrated
  2. customthe residue was partitioned between sat. NaHCO3 and EtOAc
  3. dry with materialThe organic layer was dried (MgSO4)
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-b92ddf35f0814080b320ff548fab4f2b
출처 데이터셋
uspto-grants-2007_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07238702B2

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