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

HRID 1489629노트

반응식

HRID 1489629 반응식
[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

참가 물질

6

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 211976714-(2-Tetrahydropyranyloxyethyl)-4-(3,4-dichlorophenyl)-2-pyrrolidoneHCID 21226445Aluminium lithium hydride

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
60 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-73c6ad2ffb7f4b6fbfea6c5235bbdf01
출처 데이터셋
uspto-grants-1997_10
특허 번호
US05679693

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