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 1995309ノート

反応式

HRID 1995309 の反応式
[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

参加物

5

反応物 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

生成物 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-one収率 48%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-156a1649d0e24fc5afb3aaed00bfaa85
出典データセット
uspto-grants-1983_09
特許番号
US04404138

反応ノート

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