Ethanol → HCID 22929815, 화합물

HRID 1295953노트

반응식

HRID 1295953 반응식
[C:1]([C:5]1[CH:6]=[C:7]([C:16](=[O:18])[CH3:17])[CH:8]=[C:9]([N+:13]([O-])=O)[C:10]=1[O:11][CH3:12])([CH3:4])([CH3:3])[CH3:2].[Cl-].[NH4+].C(O)C.O>[Fe].C(OCC)(=O)C>[NH2:13][C:9]1[CH:8]=[C:7]([C:16](=[O:18])[CH3:17])[CH:6]=[C:5]([C:1]([CH3:2])([CH3:3])[CH3:4])[C:10]=1[O:11][CH3:12]

참가 물질

7

반응물 4

HCID 702EthanolHCID 962WaterHCID 25517Ammonium ChlorideHCID 589100541-(3-tert-Butyl-4-methoxy-5-nitrophenyl)ethan-1-one

생성물 1

HCID 22929815HCID 22929815, 화합물수율 48.4%

시약·촉매·용매 2

HCID 23925Iron촉매HCID 8857Ethyl Acetate용매

실험 절차

Iron powder (365 g) was added to a mixture of 1-[3-(tert-butyl)-4-methoxy-5-nitrophenyl]-1-ethanone (850 g), ammonium chloride (723 g), ethanol (4 l) and water (1 l) at 70° C. to 80° C. over a period of 1 hour. The reaction mixture was cooled to room temperature and then poured into a mixture of ice water and ethyl acetate and filtered through celite. The organic layer of the mother liquor was washed with brine and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure and the resulting crystals were filtered off to yield the title compound (362 g) as white crystals.

후처리

  1. filtrationfiltered through celite
  2. washThe organic layer of the mother liquor was washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was removed under reduced pressure
  5. filtrationthe resulting crystals were filtered off

출처 및 근거

ORD 기록
ord-33a2a1170a504d928d28cf91ab1e61c5
출처 데이터셋
uspto-grants-2007_07
특허 번호
US07244730B2

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