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Methyl iodide → 4-tert-Butyl 2-methyl morpholine-2,4-dicarboxylate

HRID 456391
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반응식

HRID 456391 반응식
CI.[C:3]([O:7][C:8]([N:10]1[CH2:15][CH2:14][O:13][CH:12]([C:16]([OH:18])=[O:17])[CH2:11]1)=[O:9])([CH3:6])([CH3:5])[CH3:4].[C:19](=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[N:10]1([C:8]([O:7][C:3]([CH3:6])([CH3:4])[CH3:5])=[O:9])[CH2:15][CH2:14][O:13][CH:12]([C:16]([O:18][CH3:19])=[O:17])[CH2:11]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 27559654-((Tert-butoxy)carbonyl)morpholine-2-carboxylic acid

생성물 1

HCID 588174744-tert-Butyl 2-methyl morpholine-2,4-dicarboxylate수율 143.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Methyl iodide (9.38 ml, 150 mmol) was added to a suspension of 4-(tert-butoxycarbonyl)-2-morpholinecarboxylic acid (14.5 g, 62.6 mmol) and dry potassium carbonate (17.3 g, 125 mmol) in dry dimethylformamide (DMF) (360 ml). The mixture was stirred over night, filtered through Celite and concentrated. The residue was partitioned between dichloromethane and water. The organic phase was dried over magnesium sulfate and concentrated to give 22 g of crude product.

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후처리

  1. filtrationfiltered through Celite
  2. concentrationconcentrated
  3. customThe residue was partitioned between dichloromethane and water
  4. dry with materialThe organic phase was dried over magnesium sulfate
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-051f0f6500414de0a26c22475a10310e
출처 데이터셋
uspto-grants-2007_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07186718B2

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