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

HRID 546446

反応式

HRID 546446 の反応式
Br[CH2:2][C:3]1[N:4]=[CH:5][S:6][C:7]=1[CH2:8]Br.Cl.[CH3:11][NH:12][NH:13][CH3:14].C(N(CC)CC)C>C(O)C>[CH3:11][N:12]1[CH2:2][C:3]2[N:4]=[CH:5][S:6][C:7]=2[CH2:8][N:13]1[CH3:14]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 1344141,2-Dimethylhydrazine hydrochlorideHCID 108496984,5-Bis(bromomethyl)thiazole

生成物 1

HCID 184427415,6-Dimethyl-4,5,6,7-tetrahydrothiazolo[4,5-d]pyridazine収率 24%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
50 °C

実験手順

After 4,5-bis(bromomethyl)thiazole (600 mg) synthesized in 1) of Referential Example 109 was dissolved in ethanol (20 ml), and 1,2-dimethylhydrazine hydrochloride (294 mg) was added under ice cooling, triethylamine (1.23 ml) was added at a time, and the mixture was stirred for 30 minutes at room temperature and 30 minutes at 50° C. The solvent was distilled off, and the residue was purified by column chromatography on silica gel (methanol:dichloromethane=1:19) to obtain 5,6-dimethyl-4,5,6,7-tetrahydrothiazolo[4,5-d]-pyridazine (90 mg) as a colorless oil.

後処理

  1. distillationThe solvent was distilled off
  2. customthe residue was purified by column chromatography on silica gel (methanol:dichloromethane=1:19)

出典と根拠

ORDレコード
ord-b4ee17af7bdd4433abdf152704c4eaa8
出典データセット
uspto-grants-2011_05
特許番号
US07935824B2

関連ノート

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