4-Fluoro-3-nitrobenzotrifluoride → 1-Methyl-2-(4-trifluoromethyl-2-nitrophenoxymethyl)-5-nitro-imidazole

HRID 437582

反応式

HRID 437582 の反応式
[CH3:1][N:2]1[C:6]([N+:7]([O-:9])=[O:8])=[CH:5][N:4]=[C:3]1[CH2:10][OH:11].[N+:12]([C:15]1[CH:20]=[C:19]([C:21]([F:24])([F:23])[F:22])[CH:18]=[CH:17][C:16]=1F)([O-:14])=[O:13]>C(N(CC)CC)C>[CH3:1][N:2]1[C:6]([N+:7]([O-:9])=[O:8])=[CH:5][N:4]=[C:3]1[CH2:10][O:11][C:16]1[CH:17]=[CH:18][C:19]([C:21]([F:24])([F:22])[F:23])=[CH:20][C:15]=1[N+:12]([O-:14])=[O:13]

参加物

4

反応物 2

HCID 677784-Fluoro-3-nitrobenzotrifluorideHCID 5573562-Hydroxymethyl-1-methyl-5-nitroimidazole

生成物 1

HCID 214290871-Methyl-2-(4-trifluoromethyl-2-nitrophenoxymethyl)-5-nitro-imidazole

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

15.7 Grams (0.1 mole) of 1-methyl-2-hydroxymethyl-5-nitro-imidazole and 21.0 g (0.1 mole) of 2-nitro-4-trifluoromethylfluoro-benzene dissolved in 100 ml of butanone-2 were mixed with 15 g of triethylamine and were heated for 2 hours on a steam bath. The crystals obtained when the solution had been cooled were suction-filtered, were washed with water and were recrystallized from a little isopropanol, while adding charcoal. As a result, 25 g (= 72% of the theory) of 1-methyl-2-(4-trifluoromethyl-2-nitrophenoxymethyl)-5-nitro-imidazole were obtained in the form of yellowish crystals having a melting point of 126° C.

後処理

  1. temperaturewere heated for 2 hours on a steam bath
  2. customThe crystals obtained when the solution
  3. temperaturehad been cooled
  4. filtrationwere suction-filtered
  5. washwere washed with water
  6. customwere recrystallized from a little isopropanol
  7. additionwhile adding charcoal

出典と根拠

ORDレコード
ord-d7f13fb411254df09e955e29cf202fdc
出典データセット
uspto-grants-1977_06
特許番号
US04031232

関連ノート

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