Lithium Hydroxide → 2-Carboxy-2-(t-butyl)thiomethyl-1,2,3,4-tetrahydronaphthalene

HRID 1656046

반응식

HRID 1656046 반응식
[C:1]([C:5]1([CH2:15][S:16][C:17]([CH3:20])([CH3:19])[CH3:18])[CH2:14][CH2:13][C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH2:6]1)([O:3]C)=[O:2].[OH-].[Li+]>CO.O>[C:1]([C:5]1([CH2:15][S:16][C:17]([CH3:20])([CH3:19])[CH3:18])[CH2:14][CH2:13][C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH2:6]1)([OH:3])=[O:2]

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 197899492-Carbomethoxy-2-(t-butyl)thiomethyl-1,2,3,4-tetrahydronaphthalene

생성물 1

HCID 197899372-Carboxy-2-(t-butyl)thiomethyl-1,2,3,4-tetrahydronaphthalene수율 99%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

Dissolve 2-carbomethoxy-2-(t-butyl)thiomethyl-1,2,3,4-tetrahydronaphthalene (2.5 g, 8.6 mmol) in methanol (50 mL) and add 1N lithium hydroxide (15 mL, 15 mmol). Stir at reflux for 12 hours and at room temperature for an additional 12 hours. Dilute with water (10 mL) and concentrate in vacuo to 20 mL. Wash with ethyl ether and acidify the aqueous phase with 2N hydrochloric acid. Extract with methylene chloride (2×25 mL), dry (MgSO4) and evaporate the solvent in vacuo to give the title compound as a crystalline solid (2.37 g, 99%).

후처리

  1. concentrationconcentrate in vacuo to 20 mL
  2. washWash with ethyl ether
  3. extractionExtract with methylene chloride (2×25 mL)
  4. dry with materialdry (MgSO4)
  5. customevaporate the solvent in vacuo

출처 및 근거

ORD 기록
ord-10581ad776824abb8e98b36396b8a111
출처 데이터셋
uspto-grants-1993_10
특허 번호
US05252601

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