Triethylamine → HCID 19972853, 화합물

HRID 1077432노트

반응식

HRID 1077432 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

HCID 19972853HCID 19972853, 화합물수율 79.8%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b7f4d3893dfd4f0ea75f93e0a5460e55
출처 데이터셋
uspto-grants-1996_08
특허 번호
US05543409

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