Triethylamine → HCID 178448760、化合物
反応式
[CH2:1]([N:5]1[CH:9]=[N:8][C:7]([OH:10])=[N:6]1)[CH:2]([CH3:4])[CH3:3].C(N(CC)CC)C.[Cl:18]Cl>C(O)C>[CH2:1]([N:5]1[C:9]([Cl:18])=[N:8][C:7]([OH:10])=[N:6]1)[CH:2]([CH3:4])[CH3:3]参加物
5
実験手順
241 g of 1-isobutyl-3-hydroxy-1,2,4-triazole and 475 ml of triethylamine are dissolved in 2100 ml of absolute ethanol, and 182 g of chlorine are passed in while cooling at 20°-30°C. The solution is stirred for 1 1/4 hours at room temperature, after which the triethylamine hydrochloride is filtered off. The filtrate is concentrated in a rotary evaporator, the residue dissolved in 1000 ml of ether and 1000 ml of water are added. The phases are separated and the aqueous phase is extracted 3 times with 300 ml of ether each time. The ether phase is dried and concentrated. The residue is recrystallised from ligroin/xylene. Yield: 104.7 g (34 % of theory); m.p. 84°-86°C.
後処理
- temperaturewhile cooling at 20°-30°C
- filtrationafter which the triethylamine hydrochloride is filtered off
- concentrationThe filtrate is concentrated in a rotary evaporator
- dissolutionthe residue dissolved in 1000 ml of ether
- addition1000 ml of water are added
- customThe phases are separated
- extractionthe aqueous phase is extracted 3 times with 300 ml of ether each time
- dry with materialThe ether phase is dried
- concentrationconcentrated
- customThe residue is recrystallised from ligroin/xylene
出典と根拠
- ORDレコード
- ord-f03db375478b44fab0a4555b27a89ba0
- 出典データセット
- uspto-grants-1976_01
- 特許番号
- US03932629
反応ノート
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