Triethylamine → HCID 21190289、化合物

HRID 619468

反応式

HRID 619468 の反応式
[CH3:1][C:2]1[N:3]=[C:4]2[CH:12]=[CH:11][CH:10]=[C:9]3[N:5]2[C:6]=1[C:7](=[O:18])[N:8]3[CH2:13][CH2:14][CH2:15][CH2:16][NH2:17].C(N(CC)CC)C.[F:26][C:27]([F:35])([F:34])[C:28]([F:33])([F:32])[C:29](O)=[O:30]>C(#N)C>[CH3:1][C:2]1[N:3]=[C:4]2[CH:12]=[CH:11][CH:10]=[C:9]3[N:5]2[C:6]=1[C:7](=[O:18])[N:8]3[CH2:13][CH2:14][CH2:15][CH2:16][NH:17][C:29](=[O:30])[C:28]([F:33])([F:32])[C:27]([F:35])([F:34])[F:26]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 62356Pentafluoropropionic acidHCID 211902113-Methyl-1-[4-(amino)butan-1-yl]-1,4,7b-triazacyclopent[cd]inden-2-one

生成物 1

HCID 21190289HCID 21190289、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a solution of 2.44 g (10.0 mmol) of 3-methyl-1-[4-(amino)butan-1-yl]-1,4,7b-triazacyclopent[cd]inden-2-one and 1.81 ml (13.0 mmol) of triethylamine in 100 ml of acetonitrile was added, while stirring at room temperature, 2.31 g (12.0 mmol) of ethyl ester of pentafluoropropionic acid. The mixture was stirred for 14 hours at the same temperature. The solvent was distilled off. To the residue was added methylene chloride. The mixture was washed with water, which was dried over anhydrous magnesium sulfate. The solvent was distilled off, and the residue was purified by column chromatography (eluent:ethyl acetate), and recrystallized from ethyl acetate--hexane to afford 1.53 g (39.1%, a colorless crystals) of the desired compound.

後処理

  1. stirringThe mixture was stirred for 14 hours at the same temperature
  2. distillationThe solvent was distilled off
  3. additionTo the residue was added methylene chloride
  4. washThe mixture was washed with water, which
  5. dry with materialwas dried over anhydrous magnesium sulfate
  6. distillationThe solvent was distilled off
  7. customthe residue was purified by column chromatography (eluent:ethyl acetate)
  8. customrecrystallized from ethyl acetate
  9. customhexane to afford 1.53 g (39.1%

出典と根拠

ORDレコード
ord-302c765e62d644f081b29da537605c1f
出典データセット
uspto-grants-1999_09
特許番号
US05958942

関連ノート

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