Ethyl [(phenoxycarbonyl)oxy]acetate → 2-(Ethyloxy)-2-oxoethyl 4-[(4-bromophenyl)oxy]-1-piperidinecarboxylate

HRID 2242933ノート

反応式

HRID 2242933 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)=[CH:4][CH:3]=1.C1([O:21][C:22]([O:24][CH2:25][C:26]([O:28][CH2:29][CH3:30])=[O:27])=O)C=CC=CC=1>C1(C)C=CC=CC=1>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH:9]2[CH2:14][CH2:13][N:12]([C:22]([O:24][CH2:25][C:26]([O:28][CH2:29][CH3:30])=[O:27])=[O:21])[CH2:11][CH2:10]2)=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 12094709Ethyl [(phenoxycarbonyl)oxy]acetateHCID 126455664-(4-Bromophenoxy)piperidine

生成物 1

HCID 674168332-(Ethyloxy)-2-oxoethyl 4-[(4-bromophenyl)oxy]-1-piperidinecarboxylate収率 99.1%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
50 °C

実験手順

2.7 g (7.58 mmol) of 4-[(4-bromophenyl)-oxy]piperidine, prepared in Step 4.2, and 1.70 g (7.6 mmol) of ethyl {[(phenyloxy)carbonyl]oxy}acetate, prepared in accordance with Example 1.1, are mixed in 40 ml of toluene and the solution is heated at 50° C. for 20 hours. After cooling, it is evaporated to dryness and the product is purified by chromatography on silica gel, eluting with a 40/60 mixture of ethyl acetate and cyclohexane. The eluate is subsequently triturated in diisopropyl ether, to give 2.9 g of product in powder form.

後処理

  1. customprepared in accordance with Example 1.1
  2. temperatureAfter cooling
  3. customit is evaporated to dryness
  4. customthe product is purified by chromatography on silica gel
  5. washeluting with a 40/60 mixture of ethyl acetate and cyclohexane
  6. customThe eluate is subsequently triturated in diisopropyl ether

出典と根拠

ORDレコード
ord-81afad4f08c84058abee8c63369f8144
出典データセット
uspto-grants-2010_03
特許番号
US07674805B2

反応ノート

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