1,4-Dioxa-8-azaspiro(4.5)decane → HCID 22220290、化合物

HRID 842769ノート

反応式

HRID 842769 の反応式
F[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N+:8]([O-:10])=[O:9].[CH2:11]1[O:20][C:14]2([CH2:19][CH2:18][NH:17][CH2:16][CH2:15]2)[O:13][CH2:12]1>C1COCC1>[CH2:11]1[O:20][C:14]2([CH2:19][CH2:18][N:17]([C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=3[N+:8]([O-:10])=[O:9])[CH2:16][CH2:15]2)[O:13][CH2:12]1

参加物

4

反応物 2

HCID 674351,4-Dioxa-8-azaspiro(4.5)decaneHCID 738951-Fluoro-2-nitrobenzene

生成物 1

HCID 22220290HCID 22220290、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 1-fluoro-2-nitrobenzene (5.80 g, 41.1 mmol) and 4-piperidone ethylene ketal (6.68 g, 46.6 mmol) in THF (100 mL) was stirred at room temperature (2 h). The resulting mixture was washed with water and sodium bicarbonate solution. The aqueous layer was extracted with two portions of ethyl acetate and the combined organic extracts were washed with brine, dried over Na2SO4, and concentrated under reduced pressure. Flash chromatography on silica gel (10% ethyl acetate/hexane) afforded the title compound (7).

後処理

  1. washThe resulting mixture was washed with water and sodium bicarbonate solution
  2. extractionThe aqueous layer was extracted with two portions of ethyl acetate
  3. washthe combined organic extracts were washed with brine
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-1493041b5a2241eab151f99b99a46b08
出典データセット
uspto-grants-2002_04
特許番号
US06376503B1

反応ノート

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