Benzoyl isothiocyanate → HCID 58033240, 화합물

HRID 712175노트

반응식

HRID 712175 반응식
[Br:1][C:2]1[CH:7]=[C:6]([NH2:8])[CH:5]=[C:4]([Br:9])[N:3]=1.[C:10]([N:18]=[C:19]=[S:20])(=[O:17])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1>C1COCC1>[Br:1][C:2]1[CH:7]=[C:6]([NH:8][C:19]([NH:18][C:10](=[O:17])[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=2)=[S:20])[CH:5]=[C:4]([Br:9])[N:3]=1

참가 물질

4

반응물 2

HCID 68284Benzoyl isothiocyanate2회HCID 140910412,6-Dibromopyridin-4-amine

생성물 1

HCID 58033240HCID 58033240, 화합물수율 85%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
70 °C

실험 절차

To a solution of 2,6-dibromopyridin-4-amine in THF (250 mL) was added benzoylisothiocyanate (3.50 mL, 26.0 mmol)) and the resulting reaction mixture heated to 70° C. for 16 h. A further 1.50 mL (11.20 mmol) of benzoylisothiocyanate was added to complete the reaction and the reaction stirred at 70° C. for 16 h. After completion (by TLC), the solvent was distilled under reduced pressure, the residue treated with 10% MeOH-ether solution then filtered to obtain the desired product as a yellow solid (7.60 g, 85%).

후처리

  1. customthe resulting reaction mixture
  2. customthe reaction
  3. distillationAfter completion (by TLC), the solvent was distilled under reduced pressure
  4. additionthe residue treated with 10% MeOH-ether solution
  5. filtrationthen filtered

출처 및 근거

ORD 기록
ord-c0915ee75f7b4b318cb8f5c1f3eb47c3
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09181234B2

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