Trifluoroacetic acid → 4-(2-carboxyethyl)-2-cyclopropylmethyl-6-(3-fluoro-4-methoxyphenyl)-2H-pyridazin-3-one

HRID 982812

反応式

HRID 982812 の反応式
FC(F)(F)C(O)=O.[CH:8]1([CH2:11][N:12]2[C:17](=[O:18])[C:16]([CH2:19][CH:20](C(OC(C)(C)C)=O)[C:21]([O:23]C(C)(C)C)=[O:22])=[CH:15][C:14]([C:35]3[CH:40]=[CH:39][C:38]([O:41][CH3:42])=[C:37]([F:43])[CH:36]=3)=[N:13]2)[CH2:10][CH2:9]1>>[C:21]([CH2:20][CH2:19][C:16]1[C:17](=[O:18])[N:12]([CH2:11][CH:8]2[CH2:9][CH2:10]2)[N:13]=[C:14]([C:35]2[CH:40]=[CH:39][C:38]([O:41][CH3:42])=[C:37]([F:43])[CH:36]=2)[CH:15]=1)([OH:23])=[O:22]

参加物

3

反応物 2

HCID 6422Trifluoroacetic acidHCID 219916102-cyclopropylmethyl-4-[2,2-di(tert-butoxycarbonyl)ethyl]-6-(3-fluoro-4-methoxyphenyl)-2H-pyridazin-3-one

生成物 1

HCID 219914104-(2-carboxyethyl)-2-cyclopropylmethyl-6-(3-fluoro-4-methoxyphenyl)-2H-pyridazin-3-one収率 94.7%

実験手順

Trifluoroacetic acid (21 mL) was added to 2-cyclopropylmethyl-4-[2,2-di(tert-butoxycarbonyl)ethyl]-6-(3-fluoro-4-methoxyphenyl)-2H-pyridazin-3-one (1.39 g, 2.77 mmol), and the mixture was stirred at room temperature for 30 minutes. The solvent was distilled off under reduced pressure, and toluene was added further, followed by azeotropic boiling. The residue was heated at 190 to 200° C. for 30 minutes under a nitrogen atmosphere to yield the title compound as a pale brown powder (yield: 907 mg, 94.7%).

後処理

  1. distillationThe solvent was distilled off under reduced pressure, and toluene
  2. additionwas added further
  3. temperatureThe residue was heated at 190 to 200° C. for 30 minutes under a nitrogen atmosphere

出典と根拠

ORDレコード
ord-2bc8009a003c453186649f2b170bf1e6
出典データセット
uspto-grants-2005_03
特許番号
US06861428B2

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