Histamine → HCID 178420852, 화합물

HRID 726241

반응식

HRID 726241 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]1

참가 물질

7

반응물 4

HCID 774HistamineHCID 971Oxalic AcidHCID 3283Diethyl EtherHCID 764302-Bromothiazole

생성물 1

HCID 178420852HCID 178420852, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 3776Isopropanol용매

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

  1. concentrationThe reaction mixture is concentrated under reduced pressure until an oily residue
  2. customis obtained which
  3. customis chromatographed on a column of silica gel with a mixture of chloroform and methanol (1, 5 and 20%) as eluent
  4. customto provide an oil

출처 및 근거

ORD 기록
ord-738ccf9741894fceb21b27e96f8d0f69
출처 데이터셋
uspto-grants-1998_01
특허 번호
US05708171

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