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Acetonitrile → HCID 67070941、化合物

HRID 741938
ノート
印刷プレビュー

反応式

HRID 741938 の反応式
[F:1][C:2]1[CH:16]=[CH:15][C:5]2[C:6]([CH:9]3[CH2:14][CH2:13]NCC3)=[N:7][O:8][C:4]=2[CH:3]=1.C([O-])([O-])=O.[K+].[K+].BrCCC[CH2:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=1[O:34][CH3:35].[C:36]([OH:43])(=[O:42])/[CH:37]=[CH:38]\[C:39]([OH:41])=[O:40].[C:44](#[N:46])[CH3:45]>C(O)C>[C:36]([OH:43])(=[O:42])/[CH:37]=[CH:38]\[C:39]([OH:41])=[O:40].[F:1][C:2]1[CH:16]=[CH:15][C:5]2[C:6]([CH2:9][CH2:14][CH2:13][CH:27]([N:46]3[CH2:38][CH2:37][CH2:36][CH2:45][CH2:44]3)[C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=3[O:34][CH3:35])=[N:7][O:8][C:4]=2[CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 6342AcetonitrileHCID 11430Potassium CarbonateHCID 444266Maleic AcidHCID 8494213-(4-Piperidyl)-6-fluoro-1,2-benzisoxazoleHCID 190724681-(4-Bromobutyl)-2-methoxybenzene

生成物 1

HCID 67070941HCID 67070941、化合物

試薬・触媒・溶媒 1

HCID 702
Ethanol
溶媒

実験手順

A mixture of 6-fluoro-3-(4-piperidinyl)-1,2-benzisoxazole (2.36 g, 10.7 mmole), K2CO3 (2 g, 14.5 mmol) and 2-(4-bromobutyl)anisole (2.4 g, 10 mmol) in acetonitrile (100 ml) was heated at reflux for 2.5 hours. At the end of reaction, the solvent was removed. The residue was extracted into dichloromethane (200 ml) and filtered. The dichloromethane solution was concentrated. The crude oil obtained was purified on a flash chromatography column. The material thus purified was a light yellow oil (2.73 g, 53%). This oil was dissolved in ethanol and treated with maleic acid (607 mg, 1.0 eq) in ethanol. The 4-(6-fluoro-1,2-benzisoxazol-3-yl)-1-(2'-methoxyphenyl)-butylpiperidine maleate crystals formed on concentration and subsequent cooling to 0° C. These were collected and dried to yield 2.05 g, m.p.=132°-133° C.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 2.5 hours
  3. customAt the end of reaction
  4. customthe solvent was removed
  5. extractionThe residue was extracted into dichloromethane (200 ml)
  6. filtrationfiltered
  7. concentrationThe dichloromethane solution was concentrated
  8. customThe crude oil obtained
  9. customwas purified on a flash chromatography column
  10. customThe material thus purified
  11. dissolutionThis oil was dissolved in ethanol

出典と根拠

ORDレコード
ord-00fe3c93a90e46fab621f73e03310fb5
出典データセット
uspto-grants-1996_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05552414

反応ノート

読み込み中…

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