Triethylamine → HCID 69960946、化合物
反応式
[C:1]([C@@:4]1([OH:23])[C@@H:8]([CH:9]([C:11](=[O:13])[CH3:12])[OH:10])[O:7][C@@H:6]([N:14]2[CH:21]=[C:20]([Br:22])[C:18](=O)[NH:17][C:15]2=[O:16])[CH2:5]1)(=[O:3])[CH3:2].[CH2:24](N(CC)CC)C.C1(C)C=C(C)C=C(C)C=1S(Cl)(=O)=O.C1CCN2C(=NCCC2)CC1.[NH2:55][C:56]1[C:57]([OH:66])=[CH:58][C:59]2[C:64]([CH:65]=1)=[CH:63]C=CC=2>CN(C1C=CN=CC=1)C.C(Cl)Cl>[Br:22][C:20]1[C:18]([NH:55][C:56]2[CH:65]=[C:64]([CH3:63])[CH:59]=[C:58]([CH3:24])[C:57]=2[OH:66])=[N:17][C:15](=[O:16])[N:14]([CH:21]=1)[C@@H:6]1[O:7][C@H:8]([CH:9]([C:11](=[O:13])[CH3:12])[OH:10])[C@@:4]([C:1](=[O:3])[CH3:2])([OH:23])[CH2:5]1参加物
実験手順
To a solution of 3',5'-diacetyl-5-bromo-2'-deoxyuridine (4.0 g; 10 mmol), methylene chloride (50 ml), triethylamine (4.0 g; 40 mmol) and DMAP (0.1 g) was added 2-mesitylsulfonyl chloride (4.4 g; 20 mmol). After stirring at room temperature for 6 h. DBU (3.0 g; 20 mmol) and 3-amino-2-naphthol (6.4 g; 40 mmol) were added and the solution was stirred for 4 h. at room temperature. The reaction mixture was concentrated, the residue was dissolved in ethyl acetate and washed with saturated sodium bicarbonate aq. solution, but the title compound was precipitated from solution. The precipitates were filtered off and washed thoroughly with ethyl acetate, then methylene chloride, and dried. A small quantity of title compound also was obtained from the filtrate.
後処理
- stirringthe solution was stirred for 4 h. at room temperature
- concentrationThe reaction mixture was concentrated
- dissolutionthe residue was dissolved in ethyl acetate
- washwashed with saturated sodium bicarbonate aq. solution
- customthe title compound was precipitated from solution
- filtrationThe precipitates were filtered off
- washwashed thoroughly with ethyl acetate
- dry with materialmethylene chloride, and dried
出典と根拠
- ORDレコード
- ord-298927f3c5634edb84f6a30a1a436994
- 出典データセット
- uspto-grants-1999_12
- 特許番号
- US06005096
反応ノート
読み込み中…