Sodium Hydroxide → HCID 58033225, 화합물

HRID 447065노트

반응식

HRID 447065 반응식
C([NH:9][C:10]([NH:12][C:13]1[CH:18]=[C:17]([Br:19])[N:16]=[C:15]([Br:20])[CH:14]=1)=[S:11])(=O)C1C=CC=CC=1.[OH-].[Na+]>C1COCC1>[Br:20][C:15]1[CH:14]=[C:13]([NH:12][C:10]([NH2:9])=[S:11])[CH:18]=[C:17]([Br:19])[N:16]=1

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 58033240HCID 58033240, 화합물

생성물 1

HCID 58033225HCID 58033225, 화합물수율 87.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
62.5 °C

실험 절차

To a solution of 1-benzoyl-3-(2,6-dibromo-pyridin-4-yl)-thiourea (1.0 g, 2.14 mmol) in THF (50 mL) was added NaOH solution (0.48 in 20 mL H2O) at room temperature. The reaction mixture was heated up to 60-65° C. overnight. After completion of reaction (TLC monitoring) THF was distilled off followed by addition of water, and extraction with ethyl acetate (2×50 mL). The combined organic layers were dried over anhydrous Na2SO4, filtered and evaporated to dryness under reduced pressure. The crude residue was washed with mixture of ethyl acetate:hexane (30:70) and dried under high vacuum to get the desired product as a white solid (0.58 g, 78%).

후처리

  1. distillationwas distilled off
  2. additionfollowed by addition of water, and extraction with ethyl acetate (2×50 mL)
  3. dry with materialThe combined organic layers were dried over anhydrous Na2SO4
  4. filtrationfiltered
  5. customevaporated to dryness under reduced pressure
  6. washThe crude residue was washed with mixture of ethyl acetate:hexane (30:70)
  7. customdried under high vacuum

출처 및 근거

ORD 기록
ord-147f7f3873a04c048314a561558492fe
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08481544B2

반응 노트

불러오는 중…