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

HRID 1348780

반응식

HRID 1348780 반응식
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]

참가 물질

3

반응물 2

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

생성물 1

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

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-e258f4f492ba4cc79058a2d08367362d
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07211577B2

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