Potassium Carbonate → HCID 21453224、化合物

HRID 436601ノート

反応式

HRID 436601 の反応式
[CH2:1]([C:4]1[CH:9]=[C:8]([F:10])[CH:7]=[CH:6][C:5]=1[OH:11])[CH:2]=[CH2:3].Cl[CH2:13][CH2:14][CH2:15][N:16]1[CH2:32][CH2:31][C:19]2([N:23]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)[CH2:22][NH:21][C:20]2=[O:30])[CH2:18][CH2:17]1.C(=O)([O-])[O-].[K+].[K+]>C1(C)C=CC=CC=1>[CH2:1]([C:4]1[CH:9]=[C:8]([F:10])[CH:7]=[CH:6][C:5]=1[O:11][CH2:13][CH2:14][CH2:15][N:16]1[CH2:17][CH2:18][C:19]2([N:23]([C:24]3[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=3)[CH2:22][NH:21][C:20]2=[O:30])[CH2:31][CH2:32]1)[CH:2]=[CH2:3]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 113441122-Allyl-4-fluorophenolHCID 21453222HCID 21453222、化合物

生成物 1

HCID 21453224HCID 21453224、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of 1.5 g of 2-allyl-4-fluorophenol, 3.1 g of 8-(3-chloropropyl)-1-phenyl-4-oxo-1,3,8-triazaspiro[4,5]decane, 0.7 g of potassium carbonate and 40 ml of toluene was heated under reflux for 10 hours. After cooling, the reaction mixture was washed with water, dried over sodium sulfate and evaporated under reduced pressure. The residue was triturated with ether, cooled and filtered to give 8-{3-(2-allyl-4-fluorophenoxy)propyl}-1-phenyl-4-oxo-1,3,8-triazaspiro[4,5]decane, m.p. 110° - 113° C; recrystallized from cyclohexane, m.p. 117° - 117.5° C.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 10 hours
  3. temperatureAfter cooling
  4. washthe reaction mixture was washed with water
  5. dry with materialdried over sodium sulfate
  6. customevaporated under reduced pressure
  7. customThe residue was triturated with ether
  8. temperaturecooled
  9. filtrationfiltered

出典と根拠

ORDレコード
ord-890635a35dfe40ce913a0d17b80ad267
出典データセット
uspto-grants-1977_02
特許番号
US04009275

反応ノート

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