1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → 5-(N-(tert-butoxycarbonyl)-L-alanyl)oxy-7-methyl-3-(3-trifluoromethylphenyl)-5,6,7,8-tetrahydrocinnoline

HRID 229722

反応式

[CH3:1][CH:2]1[CH2:11][C:10]2[N:9]=[N:8][C:7]([C:12]3[CH:17]=[CH:16][CH:15]=[C:14]([C:18]([F:21])([F:20])[F:19])[CH:13]=3)=[CH:6][C:5]=2[CH:4]([OH:22])[CH2:3]1.C(N=C=NCCCN(C)C)C.[C:34]([O:38][C:39]([NH:41][C@H:42]([C:44](O)=[O:45])[CH3:43])=[O:40])([CH3:37])([CH3:36])[CH3:35]>O1CCCC1.ClCCl>[C:34]([O:38][C:39]([NH:41][C@H:42]([C:44]([O:22][CH:4]1[CH2:3][CH:2]([CH3:1])[CH2:11][C:10]2[N:9]=[N:8][C:7]([C:12]3[CH:17]=[CH:16][CH:15]=[C:14]([C:18]([F:21])([F:20])[F:19])[CH:13]=3)=[CH:6][C:5]1=2)=[O:45])[CH3:43])=[O:40])([CH3:36])([CH3:37])[CH3:35]

参加物

実験手順

7-Methyl-3-(3-trifluoromethylphenyl)-5,6,7,8-tetrahydrocinnolin-5-ol (10 mg, 0.03 mmol) obtained in Example 6 was dissolved in a mixed solvent of tetrahydrofuran and dichloromethane (0.5 mL. 0.5 mL), followed by adding N-ethyl-N′-(3-dimethylaminopropyl)carbodiimide (9 mg, 0.045 mmol), N,N-dimethylaminopyridine (catalytic amount) and N-(tert-butoxycarbonyl)-L-alanine (9 mg, 0.045 mmol) and stirring at room temperature over night. After completion of the reaction, the reaction liquid was concentrated and thus obtained residue was purified using silica gel column chromatography (hexane/ethyl acetate=1/1) to obtain an objective compound.

後処理

customAfter completion of the reaction
customthe reaction liquid
concentrationwas concentrated
customthus obtained residue was purified
customto obtain an objective compound

出典と根拠

ORDレコード: ord-17dc1c9c39fe4caa8b43c4efcbfec233
出典データセット: uspto-grants-2009_07
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US07563893B2

反応式

参加物

反応物 3

生成物 1

試薬・触媒・溶媒 2

実験手順

後処理

出典と根拠

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