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

HRID 352888

反応式

HRID 352888 の反応式
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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d27dc1db52c34ccfb27bdf9f7684590e
出典データセット
uspto-grants-2004_06
特許番号
US06747023B1

関連ノート

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