Triethylamine → HCID 19972853、化合物

HRID 1451783ノート

反応式

HRID 1451783 の反応式
C(P(C#N)(CC)=O)C.[NH2:9][CH2:10][CH:11]1[CH2:19][C:18]2[C:13](=[CH:14][CH:15]=[C:16]([C:20]3[CH:21]=[CH:22][C:23](=[O:26])[NH:24][N:25]=3)[CH:17]=2)[CH2:12]1.Br.[CH3:28][C:29]([CH3:34])=[CH:30][C:31](O)=[O:32].C(N(CC)CC)C>CN(C)C=O>[CH3:28][C:29]([CH3:34])=[CH:30][C:31]([NH:9][CH2:10][CH:11]1[CH2:19][C:18]2[C:13](=[CH:14][CH:15]=[C:16]([C:20]3[CH:21]=[CH:22][C:23](=[O:26])[NH:24][N:25]=3)[CH:17]=2)[CH2:12]1)=[O:32]

参加物

6

反応物 4

HCID 8471TriethylamineHCID 109313-Methyl-2-butenoic acidHCID 13586794DiethylphosphorylcyanideHCID 214762912-aminomethyl-5-[pyridazin-3(2H)-on-6-yl]indane hydrobromide

生成物 1

HCID 19972853HCID 19972853、化合物収率 79.8%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

Under ice cooling, 1.71 g of diethylphosphoryl cyanide was added to 80 ml of a suspension containing 3.06 g of 2-aminomethyl-5-[pyridazin-3(2H)-on-6-yl]indane·hydrobromide and 1.15 g of 3-methylcrotonic acid suspended in dimethylformamide, and then 20 ml of a solution containing 2.89 g of triethylamine dissolved in dimethylformamide was added dropwise to the mixture. The resulting mixture was stirred at the same temperature for 2.5 hours. The reaction mixture was poured into ice water, and crystals precipitated were collected by filtration. The crystals obtained were washed with water, dried and then recrystallized from ethyl acetate-methanol to obtain 2.45 g of 2-[(3-methylcrotonoyl)amino]methyl-5-[pyridazin-3(2H)-on-6-yl]indane.

後処理

  1. additionwas added dropwise to the mixture
  2. customprecipitated
  3. filtrationwere collected by filtration
  4. customThe crystals obtained
  5. washwere washed with water
  6. customdried
  7. customrecrystallized from ethyl acetate-methanol

出典と根拠

ORDレコード
ord-aef722d888424d109e975a5f148e1212
出典データセット
uspto-grants-1997_02
特許番号
US05605901

反応ノート

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