Triethylamine → 5-Nicotinoyl-Hexahydro-1H-Furo(3,4-c)Pyrrole

HRID 1283610ノート

反応式

HRID 1283610 の反応式
Cl.[C:2](Cl)(=[O:9])[C:3]1[CH:8]=[CH:7][CH:6]=[N:5][CH:4]=1.[CH2:11]1[CH:15]2[CH2:16][NH:17][CH2:18][CH:14]2[CH2:13][O:12]1.C(N(CC)CC)C>C1C=CC=CC=1>[C:2]([N:17]1[CH2:18][CH:14]2[CH2:13][O:12][CH2:11][CH:15]2[CH2:16]1)(=[O:9])[C:3]1[CH:8]=[CH:7][CH:6]=[N:5][CH:4]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 884383-Pyridinecarbonyl chloride, hydrochloride (1:1)HCID 21421150Hexahydro-1H-furo[3,4-c]pyrrole2 回

生成物 1

HCID 215185445-Nicotinoyl-Hexahydro-1H-Furo(3,4-c)Pyrrole

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

反応条件

温度
15 °C

実験手順

Nicotinoyl chloride hydrochloride, represented by formula (XII), (0.1 mole, 17.81 grams) was slowly added to a mixture of hexahydro-1H-furo(3,4-c)pyrrole, represented by formula (X), (0.1 mole, 11.3 grams), and triethylamine (0.2 mole, 20.24 grams) in 160 ml of benzene at 15°C. The reaction mixture was stirred for 1.5 hours at 15°C. and then left overnight at room temperature. The HCl salt of triethylamine was filtered and the salt was washed with benzene. The washings were combined with the filtrate and benzene was stripped under vacuum. The product, 5-nicotinoyl-hexahydro-1H-furo(3,4-c)pyrrole, represented by formula (XIII), light yellow viscous liquid, was purified by column chromatography (Alumina-eluted with methyl acetate).

後処理

  1. waitleft overnight at room temperature
  2. filtrationThe HCl salt of triethylamine was filtered
  3. washthe salt was washed with benzene
  4. customwas purified by column chromatography (Alumina-eluted with methyl acetate)

出典と根拠

ORDレコード
ord-76a60cd4b50b4fe28efe8c5fa51591bc
出典データセット
uspto-grants-1976_08
特許番号
US03975532

反応ノート

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