Ammonium Chloride → N-(3-Amino-4-trifluoromethoxy-benzyl)-2,2-dimethyl-propionamide

HRID 1258748노트

반응식

HRID 1258748 반응식
[N+:1]([C:4]1[CH:5]=[C:6]([CH:15]=[CH:16][C:17]=1[O:18][C:19]([F:22])([F:21])[F:20])[CH2:7][NH:8][C:9](=[O:14])[C:10]([CH3:13])([CH3:12])[CH3:11])([O-])=O.[NH4+].[Cl-]>[Fe].CCO>[NH2:1][C:4]1[CH:5]=[C:6]([CH:15]=[CH:16][C:17]=1[O:18][C:19]([F:20])([F:21])[F:22])[CH2:7][NH:8][C:9](=[O:14])[C:10]([CH3:13])([CH3:12])[CH3:11]

참가 물질

5

반응물 2

HCID 25517Ammonium ChlorideHCID 67975181N-(3-Nitro-4-trifluoromethoxy-benzyl)-2,2-dimethyl-propionamide

생성물 1

HCID 67975180N-(3-Amino-4-trifluoromethoxy-benzyl)-2,2-dimethyl-propionamide

시약·촉매·용매 2

HCID 23925Iron촉매HCID 702Ethanol용매

실험 절차

A mixture of N-(3-nitro-4-trifluoromethoxy-benzyl)-2,2-dimethyl-propionamide (3.4 g, 11 mmol), Fe (3.7 g, 66 mmol), saturated aqueous NH4Cl-solution (35 mL) and EtOH (170 mL) was refluxed for 30 min. The mixture was concentrated, treated with water and the pH was adjusted to ˜8. The mixture was extracted with EtOAc and the organic layer was dried over Na2SO4, filtered and concentrated. The residue was treated with PE and the sub-title compound was filtered off. Yield: 2.7 g (88%).

후처리

  1. temperaturewas refluxed for 30 min
  2. concentrationThe mixture was concentrated
  3. additiontreated with water
  4. extractionThe mixture was extracted with EtOAc
  5. dry with materialthe organic layer was dried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated
  8. additionThe residue was treated with PE
  9. filtrationthe sub-title compound was filtered off

출처 및 근거

ORD 기록
ord-9f27d2f71dab47fcb810ceb7dbe3d51b
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08466186B2

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