Nicotinic Acid → HCID 9798400, 화합물

HRID 1939913노트

반응식

HRID 1939913 반응식
CN(C)C=O.Br.[NH2:7][CH2:8][CH2:9][CH2:10][CH2:11][C:12]1[CH:17]=[CH:16][C:15]([C:18]2[CH:19]=[CH:20][C:21](=[O:24])[NH:22][N:23]=2)=[CH:14][CH:13]=1.[C:25](O)(=[O:32])[C:26]1[CH:31]=[CH:30][CH:29]=[N:28][CH:27]=1>C(N(CC)CC)C>[N:28]1[CH:29]=[CH:30][CH:31]=[C:26]([C:25]([NH:7][CH2:8][CH2:9][CH2:10][CH2:11][C:12]2[CH:13]=[CH:14][C:15]([C:18]3[CH:19]=[CH:20][C:21](=[O:24])[NH:22][N:23]=3)=[CH:16][CH:17]=2)=[O:32])[CH:27]=1

참가 물질

5

반응물 3

HCID 938Nicotinic AcidHCID 6228Dimethylformamide2회HCID 18977180HCID 18977180, 화합물

생성물 1

HCID 9798400HCID 9798400, 화합물수율 62.6%

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

Under ice cooling, a dimethylformamide solution (10 ml) containing 1.06 g of diethylphosphoric cyanide was added dropwise to a dimethylformamide suspension (30 ml) containing 1.65 g of 6-[4-(4-aminobutyl)phenyl]pyridazin-3(2H)-one hydrobromide, 0.78 g of nicotinic acid and 1.55 g of triethylamine, and the mixture was stirred for 1 hour. The reaction mixture was poured into ice water, and precipitated crystal was collected by filtration. The obtained crystal was washed with water, dried and then recrystallized from methanol to obtain 1.11 g of 6-[4-(4-(pyridin-3-ylcarbonylamino)butyl)phenyl]pyridazin-3(2H)-one.

후처리

  1. customprecipitated crystal
  2. filtrationwas collected by filtration
  3. washThe obtained crystal was washed with water
  4. customdried
  5. customrecrystallized from methanol

출처 및 근거

ORD 기록
ord-934e1b6e6f4049f78a79563c0af20c3e
출처 데이터셋
uspto-grants-1997_12
특허 번호
US05698554

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