Hydrochloric Acid → HCID 178423528、化合物
反応式
[OH-].[K+].[CH3:3][C:4]1[N:9]=[N:8][C:7]([NH:10][NH2:11])=[CH:6][CH:5]=1.[C:12](=S)=[S:13].Cl>CO>[CH3:3][C:4]1[CH:5]=[CH:6][C:7]2[N:8]([C:12]([SH:13])=[N:11][N:10]=2)[N:9]=1参加物
6
実験手順
To a solution of KOH (11.3 g, 0.202 mol) in methanol (100 mL) was added (6-methyl-pyridazin-3-yl)-hydrazine (25 g, 0.202 mol) at room temperature. The reaction mixture was placed in an ice-water bath and carbon disulfide (98 mL, 1.61 mol) was slowly added. The resultant yellow solution was heated to reflux overnight before removal of solvent. The yellow residue was acidified with 2 N aqueous HCl to pH˜4, filtered, and washed with water. Upon drying 33 g of 6-methyl-[1,2,4]triazolo[4,3-b]pyridazine-3-thiol was obtained as a yellow powder (85% yield): 1H NMR (DMSO-d6): δ 2.5 (s, 3H), 7.28 (d, 1H), 8.05 (d, 1H), 14.66 (br s, 1H); MS (m/z) 167 [M+H+]+.
後処理
- customThe reaction mixture was placed in an ice-water bath
- temperatureThe resultant yellow solution was heated
- temperatureto reflux overnight before removal of solvent
- filtrationfiltered
- washwashed with water
- dry with materialUpon drying 33 g of 6-methyl-[1,2,4]triazolo[4,3-b]pyridazine-3-thiol
出典と根拠
- ORDレコード
- ord-81c474d0a5c14922991fc6ceec5dfcda
- 出典データセット
- uspto-grants-2013_08
- 特許番号
- US08507489B2
反応ノート
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