Triethylamine → 3-[2-(2-Azabicyclo[2.2.2]oct-2-yl)ethyl]-1,2,3,4-tetrahydro-8-methoxy-5H-[1]benzopyrano[3,4-c]pyridin-5-one

HRID 1995309노트

반응식

HRID 1995309 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]2[C:9]3[CH2:14][CH2:13][NH:12][CH2:11][C:10]=3[C:15](=[O:17])[O:16][C:5]=2[CH:4]=1.C(N(CC)CC)C.Cl.Cl[CH2:27][CH2:28][N:29]1[CH2:34][CH:33]2[CH2:35][CH2:36][CH:30]1[CH2:31][CH2:32]2>O>[CH:30]12[CH2:36][CH2:35][CH:33]([CH2:32][CH2:31]1)[CH2:34][N:29]2[CH2:28][CH2:27][N:12]1[CH2:13][CH2:14][C:9]2[C:6]3[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[CH:4][C:5]=3[O:16][C:15](=[O:17])[C:10]=2[CH2:11]1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 131369188-Methoxy-1,2,3,4-tetrahydro-chromeno[3,4-c]pyridin-5-oneHCID 204881482-(2-Chloroethyl)-2-azabicyclo[2.2.2]octane hydrochloride

생성물 1

HCID 131890403-[2-(2-Azabicyclo[2.2.2]oct-2-yl)ethyl]-1,2,3,4-tetrahydro-8-methoxy-5H-[1]benzopyrano[3,4-c]pyridin-5-one수율 48%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Prepared by the method described for Example 27 from 1,2,3,4-tetrahydro-8-methoxy-5H-[1]benzopyrano[3,4-c]pyridin-5-one (3.0 g, 0.013 moles), triethylamine (3.9 ml, 0.028 moles), and 2-(2-chloroethyl)-2-azabicyclo[2.2.2]octane hydrochloride (2.9 g, 0.014 moles). Reflux time is 3 weeks. The crude product is dissolved in water, extracted with ethyl acetate, precipitated by the addition of solid potassium carbonate, filtered off, rinsed with water, and dried to yield the final product (2.3 g), mp 112°-113° C.

후처리

  1. customPrepared by the method
  2. temperatureReflux time
  3. waitis 3 weeks
  4. extractionextracted with ethyl acetate
  5. customprecipitated by the addition of solid potassium carbonate
  6. filtrationfiltered off
  7. washrinsed with water
  8. customdried

출처 및 근거

ORD 기록
ord-156a1649d0e24fc5afb3aaed00bfaa85
출처 데이터셋
uspto-grants-1983_09
특허 번호
US04404138

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