Triethylamine → HCID 69960946, 화합물
반응식
[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]1참가 물질
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-298927f3c5634edb84f6a30a1a436994
- 출처 데이터셋
- uspto-grants-1999_12
- 특허 번호
- US06005096
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