Water → 3-Tetrahydropyranyloxyethyl-3-(3,4-dichlorophenyl)pyrrolidine

HRID 727127ノート

反応式

HRID 727127 の反応式
[O:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]1[O:7][CH2:8][CH2:9][C:10]1([C:16]2[CH:21]=[CH:20][C:19]([Cl:22])=[C:18]([Cl:23])[CH:17]=2)[CH2:14][NH:13][C:12](=O)[CH2:11]1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1>[O:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]1[O:7][CH2:8][CH2:9][C:10]1([C:16]2[CH:21]=[CH:20][C:19]([Cl:22])=[C:18]([Cl:23])[CH:17]=2)[CH2:11][CH2:12][NH:13][CH2:14]1

参加物

6

反応物 4

HCID 962Water2 回HCID 14798Sodium HydroxideHCID 211976714-(2-Tetrahydropyranyloxyethyl)-4-(3,4-dichlorophenyl)-2-pyrrolidoneHCID 21226445Aluminium lithium hydride

生成物 1

HCID 211976873-Tetrahydropyranyloxyethyl-3-(3,4-dichlorophenyl)pyrrolidine収率 90.7%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
60 °C

実験手順

3.9 g of the 4-(2-tetrahydropyranyloxyethyl)-4-(3,4-dichlorophenyl)-2-pyrrolidone prepared above are dissolved in 50 ml of tetrahydrofuran and the solution is added to a suspension of 0.9 g of lithium aluminum hydride in 5 ml of THF heated to 60° C. The reaction mixture is heated for one hour at 60° C. and then cooled. 1 ml of water, 1 ml of 4N sodium hydroxide and 3 ml of water are added. The inorganic material is filtered off and the filtrate is concentrated under vacuum. The residue is taken up in ethyl ether, dried over MgSO4 and concentrated under vacuum to give 3.4 g of the expected product.

後処理

  1. temperatureThe reaction mixture is heated for one hour at 60° C.
  2. temperaturecooled
  3. filtrationThe inorganic material is filtered off
  4. concentrationthe filtrate is concentrated under vacuum
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-b456e97c223f49eeaec2596e6e146a26
出典データセット
uspto-grants-1998_01
特許番号
US05712288

反応ノート

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