反応式
C([N:8]1[CH2:31][CH2:30][C:11]2[N:12]=[CH:13][N:14]=[C:15]([NH:16][C:17]3[CH:22]=[CH:21][C:20]([S:23]([C:26]([F:29])([F:28])[F:27])(=[O:25])=[O:24])=[CH:19][CH:18]=3)[C:10]=2[CH2:9]1)C1C=CC=CC=1.ClC(OC(Cl)=O)C.C(N(CC)C(C)C)(C)C>C(Cl)(Cl)Cl>[F:29][C:26]([F:27])([F:28])[S:23]([C:20]1[CH:21]=[CH:22][C:17]([NH:16][C:15]2[C:10]3[CH2:9][NH:8][CH2:31][CH2:30][C:11]=3[N:12]=[CH:13][N:14]=2)=[CH:18][CH:19]=1)(=[O:24])=[O:25]参加物
5
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
6-Benzyl-5,6,7,8-tetrahydro-N-(4-(trifluoromethylsulfonyl)phenyl)pyrido[4,3-d]pyrimidin-4-amine (270 mg, 0.55 mmol) was dissolved in anhydrous chloroform (10 mL) and 1-chloroethylchloroformate was added (0.18 mL, 1.65 mmol). After stirring for 30 min, N,N-diisopropylethylamine was added (0.24 mL, 1.65 mmol) and the mixture was stirred for an additional 2 h. The chloroform was removed under vacuum and 30 ml of methanol was added and the mixture was heated for 30 min. Upon reaction completion, the methanol was removed and the residue was dissolved in ethyl acetate and washed with sat. NaHCO3 and brine. The organic layer was dried over Na2SO4, filtered and evaporated to give the product (163 mg, 83%).
後処理
- stirringthe mixture was stirred for an additional 2 h
- customThe chloroform was removed under vacuum and 30 ml of methanol
- additionwas added
- temperaturethe mixture was heated for 30 min
- customUpon reaction completion
- customthe methanol was removed
- dissolutionthe residue was dissolved in ethyl acetate
- washwashed with sat. NaHCO3 and brine
- dry with materialThe organic layer was dried over Na2SO4
- filtrationfiltered
- customevaporated
出典と根拠
- ORDレコード
- ord-4801c6f6649e49269c71b088f756b648
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07745451B2
関連ノート
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