Ethanol → HCID 22929815、化合物

HRID 1295953ノート

反応式

HRID 1295953 の反応式
[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]

参加物

7

反応物 4

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

生成物 1

HCID 22929815HCID 22929815、化合物収率 48.4%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-33a2a1170a504d928d28cf91ab1e61c5
出典データセット
uspto-grants-2007_07
特許番号
US07244730B2

反応ノート

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