反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([Cl:11])[CH:10]=1)[C:5]([OH:7])=O.[CH3:12][CH2:13]N(C(C)C)C(C)C.Cl.Cl.[NH2:23][CH2:24][CH:25]1[CH2:30][CH2:29][N:28]([CH2:31][CH2:32][NH:33][S:34]([C:37](F)(F)F)(=[O:36])=[O:35])[CH2:27][CH2:26]1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F>CN(C=O)C>[Cl:11][C:9]1[CH:8]=[C:4]([CH:3]=[C:2]([Cl:1])[CH:10]=1)[C:5]([NH:23][CH2:24][CH:25]1[CH2:30][CH2:29][N:28]([CH2:31][CH2:32][NH:33][S:34]([CH:37]2[CH2:13][CH2:12]2)(=[O:36])=[O:35])[CH2:27][CH2:26]1)=[O:7]参加物
6
反応物 4
HCID 58113,5-Dichlorobenzoic acid
HCID 81531Diisopropylethylamine
HCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)
HCID 67029054N-(2-(4-(aminomethyl)piperidin-1-yl)ethyl)-1,1,1-trifluoromethanesulfonamide dihydrochloride salt生成物 1
試薬・触媒・溶媒 1
実験手順
To a solution of 3,5-dichlorobenzoic acid (23 mg, 0.12 mmol) in DMF (2 mL) was added DIPEA (0.1 mL, 0.6 mmol), N-(2-(4-(aminomethyl) piperidin-1-yl)ethyl)-1,1,1-trifluoromethanesulfonamide dihydrochloride salt (40 mg, 0.12 mmol) and HATU (60 mg, 0.15 mmol). The reaction mixture was stirred at room temperature overnight. The organic layer was washed with sat. NaHCO3 aq. (8 mL), dried over Na2SO4, and concentrated to give crude product which was subsequently purified by High Throughput Purification System (HiTOPs).
後処理
- washThe organic layer was washed with sat. NaHCO3 aq. (8 mL)
- dry with materialdried over Na2SO4
- concentrationconcentrated
- customto give crude product which
- customwas subsequently purified by High Throughput Purification System (HiTOPs)
出典と根拠
- ORDレコード
- ord-95ddbb57b44e497b93f652b7f4af4773
- 出典データセット
- uspto-grants-2013_02
- 特許番号
- US08377968B2
関連ノート
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