Lithium Hydroxide → HCID 21017824, 화합물

HRID 644939

반응식

HRID 644939 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C@@H:8]2[CH2:13][CH2:12][C:11](=[O:14])[CH2:10][C@H:9]2[C:15]([O:17]C)=[O:16])=[CH:4][CH:3]=1.[OH-].[Li+].Cl.[Cl-].[Na+].O>O1CCCC1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C@@H:8]2[CH2:13][CH2:12][C:11](=[O:14])[CH2:10][C@H:9]2[C:15]([OH:17])=[O:16])=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 3939Lithium HydroxideHCID 68520286Methyl trans-2-(4-chlorophenyl)-5-oxocyclohexanecarboxylateHCID 131718760Hydrochloric acid brine

생성물 1

HCID 21017824HCID 21017824, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A stirred mixture of 0.435 g (1.63 mmol) of methyl trans-2-(4-chlorophenyl)-5-oxocyclohexanecarboxylate (described in Step B of Example 1) and 1 N lithium hydroxide (3.26 mL, 3.26 mmol) in tetrahydrofuran (3.3 mL) was heated at reflux for approximately 1 h. After cooling to room temperature, the reaction mixture was poured into 1 N hydrochloric acid/brine (1:1) and extracted three times with methylene chloride. The combined organic extracts were washed with brine, dried (MgSO4) and concentrated in vacuo. The residual crude title compound was used without further purification in the subsequent reaction.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for approximately 1 h
  3. extractionextracted three times with methylene chloride
  4. washThe combined organic extracts were washed with brine
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated in vacuo
  7. customThe residual crude title compound was used without further purification in the subsequent reaction

출처 및 근거

ORD 기록
ord-1efd9cc470724fba99bfaf4fda84b551
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07700778B2

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