Histamine → HCID 178420852、化合物
反応式
[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]1参加物
7
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-738ccf9741894fceb21b27e96f8d0f69
- 出典データセット
- uspto-grants-1998_01
- 特許番号
- US05708171
反応ノート
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