Nicotinic Acid → HCID 9798400、化合物

HRID 1939913ノート

反応式

HRID 1939913 の反応式
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

参加物

5

反応物 3

HCID 938Nicotinic AcidHCID 6228Dimethylformamide2 回HCID 18977180HCID 18977180、化合物

生成物 1

HCID 9798400HCID 9798400、化合物収率 62.6%

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-934e1b6e6f4049f78a79563c0af20c3e
出典データセット
uspto-grants-1997_12
特許番号
US05698554

反応ノート

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