Sodium Hydroxide → HCID 20340740、化合物

HRID 1076244ノート

反応式

HRID 1076244 の反応式
O[CH2:2][CH2:3][CH2:4][C:5]1[N:13]=[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][N:7]2[N:6]=1.P(Cl)(Cl)([Cl:16])=O.[OH-].[Na+]>C(Cl)(Cl)Cl>[Cl:16][CH2:2][CH2:3][CH2:4][C:5]1[N:13]=[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][N:7]2[N:6]=1

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 24813Phosphorus oxychlorideHCID 20340747HCID 20340747、化合物

生成物 1

HCID 20340740HCID 20340740、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

To a solution of 34.5g of 2-(3-hydroxypropyl)-s-triazolo-[1,5-a]pyridine in 500 ml of chloroform is added dropwise 77g of phosphorous oxychloride at a temperature of from 5° to 15°C. After the addition is completed, the reaction mixture is heated on a water bath for 1 hr. and then added to 300 g of ice-water. The mixture is then treated with an aqueous sodium hydroxide solution. Then the organic layer is separated from the aqueous layer, dried over anhydrous sodium sulfate and concentrated to give the residue, which is chromatographed over alumina with benzene. Twenty-three grams of 2-(3-chloropropyl)-s-triazolo[1,5-a]pyridine are obtained as colorless needles after recrystallization from cyclohexane, melting point 56.5°-57°C.

後処理

  1. additionAfter the addition
  2. temperaturethe reaction mixture is heated on a water bath for 1 hr
  3. customThen the organic layer is separated from the aqueous layer
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated
  6. customto give the residue, which
  7. customis chromatographed over alumina with benzene

出典と根拠

ORDレコード
ord-bd3c24cddbf7480cb8229d47b53f7141
出典データセット
uspto-grants-1976_05
特許番号
US03956328

反応ノート

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