Ammonium Hydroxide → 5-(3-Methylpentan-3-yl)-1,3,4-thiadiazol-2-amine

HRID 1649313

반응식

HRID 1649313 반응식
[CH2:1]([C:3]([CH3:9])([CH2:7][CH3:8])[C:4](O)=O)[CH3:2].[NH2:10][NH:11][C:12]([NH2:14])=[S:13].P(Cl)(Cl)(Cl)=O.[OH-].[NH4+]>O1CCOCC1>[NH2:14][C:12]1[S:13][C:4]([C:3]([CH2:7][CH3:8])([CH3:9])[CH2:1][CH3:2])=[N:10][N:11]=1

참가 물질

6

반응물 4

HCID 14923Ammonium HydroxideHCID 24813Phosphorus oxychlorideHCID 298462-Ethyl-2-methylbutyric acidHCID 2723789Thiosemicarbazide

생성물 1

HCID 132342635-(3-Methylpentan-3-yl)-1,3,4-thiadiazol-2-amine수율 91.9%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
90 °C

실험 절차

A solution containing 13.0 g of 2-ethyl-2-methylbutyric acid and 9.1 g of thiosemicarbazide in 125 ml of dioxane was stirred and heated to 90° C. To the stirred reaction mixture was added dropwise over thirty minutes 15.3 g of phosphorous oxychloride. Following complete addition, the reaction mixture was heated at 90° C. for six hours. The mixture was then cooled to about 30° C. and added to 100 g of ice. The aqueous mixture was made alkaline by the addition of ammonium hydroxide, and the alkaline solution was extracted several times with ethyl acetate. The extracts were combined, washed with water, dried, and the solvent was removed by evaporation under reduced pressure to afford 17.0 g of 2-amino-5-(1-ethyl-1-methylpropyl)-1,3,4-thiadiazole.

후처리

  1. customTo the stirred reaction mixture
  2. additionaddition
  3. temperaturethe reaction mixture was heated at 90° C. for six hours
  4. temperatureThe mixture was then cooled to about 30° C.
  5. extractionthe alkaline solution was extracted several times with ethyl acetate
  6. washwashed with water
  7. customdried
  8. customthe solvent was removed by evaporation under reduced pressure

출처 및 근거

ORD 기록
ord-a84f06af9dff452c90b10adf40dd1c5d
출처 데이터셋
uspto-grants-1983_11
특허 번호
US04416683

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