Diisopropyl Ether → HCID 19431474, 화합물

HRID 1451781노트

반응식

HRID 1451781 반응식
C(N(CC)CC)C.[NH2:8][CH:9]1[CH2:17][C:16]2[C:11](=[CH:12][CH:13]=[C:14]([C:18]3[CH:19]=[CH:20][C:21](=[O:24])[NH:22][N:23]=3)[CH:15]=2)[CH2:10]1.Br.[CH2:26]([N:29]=[C:30]=[S:31])[CH2:27][CH3:28].C(OC(C)C)(C)C>COCCO.O>[CH2:26]([NH:29][C:30]([NH:8][CH:9]1[CH2:17][C:16]2[C:11](=[CH:12][CH:13]=[C:14]([C:18]3[CH:19]=[CH:20][C:21](=[O:24])[NH:22][N:23]=3)[CH:15]=2)[CH2:10]1)=[S:31])[CH2:27][CH3:28]

참가 물질

7

반응물 4

HCID 7914Diisopropyl EtherHCID 8471TriethylamineHCID 69403Propyl IsothiocyanateHCID 189297722-amino-5-[pyridazin-3(2H)-on-6-yl]indane hydrobromide

생성물 1

HCID 19431474HCID 19431474, 화합물수율 84.3%

시약·촉매·용매 2

HCID 962Water용매HCID 80192-Methoxyethanol용매

실험 절차

Triethylamine (2.0 g) was added to 60 ml of a suspension containing 5.04 g of 2-amino-5-[pyridazin-3(2H)-on-6-yl]indane·hydrobromide suspended in 2-methoxyethanol, and the mixture was stirred for 10 minutes. Then, 2.33 g of propyl isothiocyanate was added dropwise to the mixture, and the resulting mixture was stirred at 50° C. for 7 hours. After cooling, 100 ml of water and 300 ml of isopropyl ether were added to the reaction mixture, and the resulting mixture was stirred. Crystals precipitated were collected by filtration, washed with water and dried. The crystals obtained were recrystallized from ethanol to obtain 4.53 g of 2-[(propyl) thiocarbamoyl]amino-5-[pyridazin-3(2H)-on-6-yl]indane.

후처리

  1. stirringthe resulting mixture was stirred at 50° C. for 7 hours
  2. temperatureAfter cooling
  3. stirringthe resulting mixture was stirred
  4. customCrystals precipitated
  5. filtrationwere collected by filtration
  6. washwashed with water
  7. customdried
  8. customThe crystals obtained
  9. customwere recrystallized from ethanol

출처 및 근거

ORD 기록
ord-a106d8ca84f547e481e6a3a916d24315
출처 데이터셋
uspto-grants-1997_02
특허 번호
US05605901

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