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Methyl iodide → 4-(Tert-butoxy)-3-methyl-4-oxobutanoic acid

HRID 1469655
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HRID 1469655 반응식
[Li+].[CH3:2]C([N-]C(C)C)C.[C:9]([O:13][C:14](=[O:20])[CH2:15][CH2:16][C:17]([OH:19])=[O:18])([CH3:12])([CH3:11])[CH3:10].CI>C1COCC1>[C:9]([O:13][C:14](=[O:20])[CH:15]([CH3:2])[CH2:16][C:17]([OH:19])=[O:18])([CH3:12])([CH3:10])[CH3:11]
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참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 2724682Lithium diisopropylamideHCID 41391074-(Tert-butoxy)-4-oxobutanoic acid

생성물 1

HCID 127614644-(Tert-butoxy)-3-methyl-4-oxobutanoic acid

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
-20 °C

실험 절차

To a stirred solution of LDA (6.3 mmol, 2M in hexane) in THF (5 mL) at −78° C. is added a solution of succinic acid mono-tert-butyl ester (523 mg, 3 mmol) in THF (2 mL) dropwise. After the addition, the mixture is warmed to −20° C. slowly and stirred at −20° C. for 30 minutes. The solution is re-cooled to −78° C. and MeI (511 mg, 3.6 mmol) is added dropwise. The mixture is warmed to room temperature and stirred for 18 hours. The mixture is quenched with water and extracted with ethyl acetate. The organic layer is washed with water, brine, dried over MgSO4 and filtered. The solvent is removed under reduced pressure to give 2-methyl-succinic acid 1-tert-butyl ester.

후처리

  1. additionAfter the addition
  2. temperatureThe solution is re-cooled to −78° C.
  3. temperatureThe mixture is warmed to room temperature
  4. stirringstirred for 18 hours
  5. customThe mixture is quenched with water
  6. extractionextracted with ethyl acetate
  7. washThe organic layer is washed with water, brine
  8. dry with materialdried over MgSO4
  9. filtrationfiltered
  10. customThe solvent is removed under reduced pressure

출처 및 근거

ORD 기록
ord-af28f5bea6b24a6d801882b8c216124b
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09006249B2

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