Triethylamine → 5,6-Dimethyl-4,5,6,7-tetrahydrothiazolo[4,5-d]pyridazine

HRID 352888

반응식

HRID 352888 반응식
Br[CH2:2][C:3]1[N:4]=[CH:5][S:6][C:7]=1[CH2:8]Br.Cl.Cl.[CH3:12][NH:13][NH:14][CH3:15].C(N(CC)CC)C>C(O)C>[CH3:12][N:13]1[CH2:2][C:3]2[N:4]=[CH:5][S:6][C:7]=2[CH2:8][N:14]1[CH3:15]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 93801,2-Dimethylhydrazine dihydrochlorideHCID 108496984,5-Bis(bromomethyl)thiazole

생성물 1

HCID 184427415,6-Dimethyl-4,5,6,7-tetrahydrothiazolo[4,5-d]pyridazine

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Under ice cooling, 4,5-bis(bromomethyl)thiazole (600 mg) and 1,2-dimethylhydrazine dihydrochloride (294 mg) were suspended in ethanol (20 ml). Triethylamine (1.23 ml) was added in one portion to the reaction mixture, followed by stirring at room temperature for 30 minutes and then, at 50° C. for 30 minutes. The solvent was distilled off and the residue was purified by chromatography on a silica gel column (5% methanol—methylene chloride), whereby the title compound (90 mg, 24%) was obtained.

후처리

  1. waitat 50° C. for 30 minutes
  2. distillationThe solvent was distilled off
  3. customthe residue was purified by chromatography on a silica gel column (5% methanol—methylene chloride), whereby the title compound (90 mg, 24%)
  4. customwas obtained

출처 및 근거

ORD 기록
ord-d27dc1db52c34ccfb27bdf9f7684590e
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06747023B1

연결된 노트

불러오는 중…