反応式
CCN(C(C)C)C(C)C.[N:10]1([C:14]([C:16]2[CH:43]=[CH:42][C:19]([O:20][C:21]3[CH:22]=[C:23]([CH:27]=[C:28]([O:30][C@@H:31]([CH3:41])[CH2:32][O:33][Si:34]([C:37]([CH3:40])([CH3:39])[CH3:38])([CH3:36])[CH3:35])[CH:29]=3)[C:24](O)=[O:25])=[CH:18][CH:17]=2)=[O:15])[CH2:13][CH2:12][CH2:11]1.[NH2:44][C:45]1[CH:49]=[C:48]([CH3:50])[N:47]([CH3:51])[N:46]=1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F>CN(C=O)C.O>[N:10]1([C:14]([C:16]2[CH:43]=[CH:42][C:19]([O:20][C:21]3[CH:22]=[C:23]([CH:27]=[C:28]([O:30][C@@H:31]([CH3:41])[CH2:32][O:33][Si:34]([C:37]([CH3:38])([CH3:39])[CH3:40])([CH3:36])[CH3:35])[CH:29]=3)[C:24]([NH:44][C:45]3[CH:49]=[C:48]([CH3:50])[N:47]([CH3:51])[N:46]=3)=[O:25])=[CH:18][CH:17]=2)=[O:15])[CH2:11][CH2:12][CH2:13]1参加物
7
反応物 4
HCID 81531Diisopropylethylamine
HCID 70177471,5-dimethyl-1H-pyrazol-3-amine
HCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)
HCID 593468963-[4-(Azetidin-1-ylcarbonyl)phenoxy]-5-((1S)-2-{[tert-butyl(dimethyl)silyl]oxy}-1-methylethoxy)benzoic acid生成物 1
試薬・触媒・溶媒 2
実験手順
DIPEA (517 mg, 3.00 mmol) was added to a solution of 3-[4-(azetidin-1-ylcarbonyl)phenoxy]-5-((1S)-2-{[tert-butyl(dimethyl)silyl]oxy}-1-methylethoxy)benzoic acid (364 mg, 0.75 mmol), 3-amino-1,5-dimethylpyrazole (109 mg, 0.90 mmol) and HATU (599 mg, 1.58 mmol) in DMF (3.0 mL) and the mixture stirred for 24 hours. Water (25 mL) was added and the mixture extracted with ethyl acetate (2×25 mL) dried (MgSO4) and reduced to a brown oil. The crude product was purified by chromatography on silica, eluting with ethyl acetate, to give the required product as a clear oil. (232 mg).
後処理
- extractionthe mixture extracted with ethyl acetate (2×25 mL)
- dry with materialdried (MgSO4)
- customThe crude product was purified by chromatography on silica
- washeluting with ethyl acetate
出典と根拠
- ORDレコード
- ord-77da95266a1440d4ba6ebc2834eee542
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07745475B2
関連ノート
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