Ethanol → 2-Amino-5-chloro-8-methoxy[1,2,4]triazolo[1,5-a]pyridine

HRID 1940928ノート

反応式

HRID 1940928 の反応式
Cl.NO.C([N:7](C(C)C)CC)(C)C.C(O)C.[Cl:16][C:17]1[N:22]=[C:21]([NH:23][C:24]([NH:26]C(OCC)=O)=S)[C:20]([O:32][CH3:33])=[CH:19][CH:18]=1>O>[NH2:7][C:24]1[N:23]=[C:21]2[C:20]([O:32][CH3:33])=[CH:19][CH:18]=[C:17]([Cl:16])[N:22]2[N:26]=1

参加物

6

反応物 4

HCID 702EthanolHCID 81531DiisopropylethylamineHCID 443297Hydroxyamine hydrochlorideHCID 21464341N-(6-Chloro-3-methoxy-2-pyridinyl)-N'-carboethoxythiourea

生成物 1

HCID 183661952-Amino-5-chloro-8-methoxy[1,2,4]triazolo[1,5-a]pyridine収率 58.6%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Hydroxylamine hydrochloride (9.6 g, 138 mmol) and diisopropylethylamine (14.4 mL, 10.7 g, 83 mmol) were mixed with ethanol (300 mL) for a few minutes and then N-(6-chloro-3-methoxy-2-pyridinyl)-N'-carboethoxythiourea (7.6 g, 27.5 mmol) was added with stirring. The resulting mixture was stirred at room temperature for 20 min and then heated to reflux for 3 hours. The volatile components were removed by evaporation and the residue obtained was mixed with water. The resulting slurry was filtered and the solids collected were washed with ether, a small amount of methanol, and finally hexane and were then dried. The title compound (3.2 g) was obtained as a tan powder melting at 207°-208° C.

後処理

  1. stirringThe resulting mixture was stirred at room temperature for 20 min
  2. temperatureheated
  3. temperatureto reflux for 3 hours
  4. customThe volatile components were removed by evaporation
  5. customthe residue obtained
  6. filtrationThe resulting slurry was filtered
  7. customthe solids collected
  8. washwere washed with ether
  9. dry with materiala small amount of methanol, and finally hexane and were then dried

出典と根拠

ORDレコード
ord-2e93278c6de64f08ad22b94276dcdead
出典データセット
uspto-grants-1997_12
特許番号
US05700940

反応ノート

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