Sodium Carbonate → 4-(Propan-2-yl)-1,3-thiazol-2-amine

HRID 532491

반응식

HRID 532491 반응식
Br[CH2:2][C:3](=O)[CH:4]([CH3:6])[CH3:5].[NH2:8][C:9]([NH2:11])=[S:10].C(=O)([O-])[O-].[Na+].[Na+]>C(O)C>[CH:4]([C:3]1[N:8]=[C:9]([NH2:11])[S:10][CH:2]=1)([CH3:6])[CH3:5]

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 2723790ThioureaHCID 108990371-Bromo-3-methylbutan-2-one

생성물 1

HCID 70640774-(Propan-2-yl)-1,3-thiazol-2-amine수율 69.8%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
60 °C

실험 절차

2 g of 1-bromo-3-methyl-butan-2-one obtained in step 93-1 was added to 20 ml of ethanol and 920 mg of thiourea was added thereto. The mixture was heated to 60° C., stirred for 3.5 hr and cooled to room temperature. The resulting mixture was added with aqueous sodium carbonate and extracted twice with ethyl acetate. The organic layer was washed with water and saline solution, dried over anhydrous magnesium sulfate and concentrated under a reduced pressure. The resulting residue thus obtained was purified by column chromatography (ethyl acetate/hexane=1/2) to obtain 1.2 g of the title compound.

후처리

  1. additionwas added
  2. temperaturecooled to room temperature
  3. extractionextracted twice with ethyl acetate
  4. washThe organic layer was washed with water and saline solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated under a reduced pressure
  7. customThe resulting residue thus obtained
  8. customwas purified by column chromatography (ethyl acetate/hexane=1/2)

출처 및 근거

ORD 기록
ord-596310d4f0054dd4a6af4e7f044e023b
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08853213B2

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