反応式
C(N(CC)C(C)C)(C)C.[C:10]([O:14][C:15]([N:17]1[CH2:21][CH2:20][CH:19]([C:22]([OH:24])=O)[CH2:18]1)=[O:16])([CH3:13])([CH3:12])[CH3:11].CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.Cl.[NH2:50][CH2:51][C:52]([C:54]1[CH:59]=[CH:58][C:57]([Br:60])=[CH:56][CH:55]=1)=[O:53]>CN(C=O)C>[C:10]([O:14][C:15]([N:17]1[CH2:21][CH2:20][CH:19]([C:22](=[O:24])[NH:50][CH2:51][C:52]([C:54]2[CH:59]=[CH:58][C:57]([Br:60])=[CH:56][CH:55]=2)=[O:53])[CH2:18]1)=[O:16])([CH3:11])([CH3:12])[CH3:13]参加物
7
反応物 5
HCID 313Hydrochloric Acid
HCID 216392-Amino-1-(4-bromophenyl)ethanone
HCID 81531Diisopropylethylamine
HCID 27605291-((Tert-butoxy)carbonyl)pyrrolidine-3-carboxylic acid
HCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)生成物 1
試薬・触媒・溶媒 1
実験手順
N,N-diisopropylethylamine (5.3 mL, 30.6 mmol) was added dropwise to a mixture of pyrrolidine-1,3-dicarboxylic acid 1-tert-butyl ester (2.2 g, 10.1 mmol), HATU (4.0 g, 10.5 mmol), the HCl salt of 2-amino-1-(4-bromophenyl)ethanone (2.4 g, 9.6 mmol), and DMF (40 mL), and stirred at ambient condition for 1 hour. Most of the volatile component was removed in vacuo, and the resulting residue was dissolved in ethyl acetate (150 mL), washed with water and brine, dried over Na2SO4, filtered and concentrated in vacuo. The obtained residue was purified by flash chromatography to provide the desired product as a white foam-like solid (3.5 g, 90%). m/z 432.9, 434.9 (M+Na)+.
後処理
- customMost of the volatile component was removed in vacuo
- dissolutionthe resulting residue was dissolved in ethyl acetate (150 mL)
- washwashed with water and brine
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe obtained residue was purified by flash chromatography
出典と根拠
- ORDレコード
- ord-0baad03097534a28b6b5b4bc17b31fd3
- 出典データセット
- uspto-grants-2012_01
- 特許番号
- US08088368B2
関連ノート
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