Sodium Hydroxide → HCID 20340740, 화합물

HRID 1076244노트

반응식

HRID 1076244 반응식
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

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 24813Phosphorus oxychlorideHCID 20340747HCID 20340747, 화합물

생성물 1

HCID 20340740HCID 20340740, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-bd3c24cddbf7480cb8229d47b53f7141
출처 데이터셋
uspto-grants-1976_05
특허 번호
US03956328

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