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

HRID 1283610노트

반응식

HRID 1283610 반응식
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

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 884383-Pyridinecarbonyl chloride, hydrochloride (1:1)HCID 21421150Hexahydro-1H-furo[3,4-c]pyrrole2회

생성물 1

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

시약·촉매·용매 1

HCID 241Benzene용매

반응 조건

온도
15 °C

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-76a60cd4b50b4fe28efe8c5fa51591bc
출처 데이터셋
uspto-grants-1976_08
특허 번호
US03975532

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