Sodium Hydroxide → Methyl (4-iodo-5-methylpyridin-2-yl)carbamate

HRID 537032노트

반응식

HRID 537032 반응식
[CH3:1][O:2][C:3]([N:5]([C:10]1[CH:15]=[C:14]([I:16])[C:13]([CH3:17])=[CH:12][N:11]=1)C(OC)=O)=[O:4].[OH-].[Na+]>CO>[CH3:1][O:2][C:3](=[O:4])[NH:5][C:10]1[CH:15]=[C:14]([I:16])[C:13]([CH3:17])=[CH:12][N:11]=1

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 66748316Dimethyl(4-iodo-5-methylpyridin-2-yl)imidodicarbonate

생성물 1

HCID 67952848Methyl (4-iodo-5-methylpyridin-2-yl)carbamate수율 75.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Dimethyl(4-iodo-5-methylpyridin-2-yl)imidodicarbonate (110 g, 310 mmol) was added to a mixture of MeOH (1500 mL) and 1M NaOH (620 mL). The reaction mixture was allowed to stir at rt for 1.5 h and was then concentrated. EtOAc and water were added to the residue and the solution was extracted with EtOAc. The organic solutions were combined, washed with brine, dried over Na2SO4, filtered and concentrated to give methyl(4-iodo-5-methylpyridin-2-yl)carbamate (68 g, 60%) which was used in the next step without purification.

후처리

  1. concentrationwas then concentrated
  2. additionEtOAc and water were added to the residue
  3. extractionthe solution was extracted with EtOAc
  4. washwashed with brine
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-8de1e3babf17429e99ca7dcda2c8e749
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08859768B2

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