Nicotinic Acid → HCID 9798400、化合物

HRID 2393737ノート

反応式

HRID 2393737 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-5b5a710aa42842b497bad362832de5f0
出典データセット
uspto-grants-1998_09
特許番号
US05808065

反応ノート

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