Histamine → HCID 178420852, 화합물
반응식
[CH:1]1[N:5]=[CH:4][NH:3][C:2]=1[CH2:6][CH2:7][NH2:8].Br[C:10]1[S:11][CH:12]=[CH:13][N:14]=1.C(O)(=O)C(O)=O.CCOCC>CC(O)C.C(O)C>[NH:5]1[CH:1]=[C:2]([CH2:6][CH2:7][NH:8][C:10]2[S:11][CH:12]=[CH:13][N:14]=2)[N:3]=[CH:4]1참가 물질
7
실험 절차
1.1 g (10 mmol) of histamine base and 1.6 g (10 mmol) of 2-bromothiazole are brought to reflux in 15 ml of 2-propanol for 96 h. The reaction mixture is concentrated under reduced pressure until an oily residue is obtained which is chromatographed on a column of silica gel with a mixture of chloroform and methanol (1, 5 and 20%) as eluent to provide an oil. The latter is taken up in absolute ethanol and is treated with oxalic acid (2 molar equivalents). Addition of ether gives the title compound in the dioxalate form which, after having been crystallized from 2-propanol, melts at 198°-199° C.
후처리
- concentrationThe reaction mixture is concentrated under reduced pressure until an oily residue
- customis obtained which
- customis chromatographed on a column of silica gel with a mixture of chloroform and methanol (1, 5 and 20%) as eluent
- customto provide an oil
출처 및 근거
- ORD 기록
- ord-738ccf9741894fceb21b27e96f8d0f69
- 출처 데이터셋
- uspto-grants-1998_01
- 특허 번호
- US05708171
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