Ethyl chloroformate → HCID 86717590, 화합물

HRID 715527

반응식

HRID 715527 반응식
[CH3:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[N:5]=[CH:4][C:3]=1[NH2:10].Cl[C:12]([O:14][CH2:15][CH3:16])=[O:13]>N1C=CC=CC=1>[CH3:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[N:5]=[CH:4][C:3]=1[NH:10][C:12](=[O:13])[O:14][CH2:15][CH3:16]

참가 물질

4

반응물 2

HCID 10928Ethyl chloroformateHCID 2431706-Methoxy-4-methylpyridin-3-amine

생성물 1

HCID 86717590HCID 86717590, 화합물수율 94.6%

시약·촉매·용매 1

HCID 1049Pyridine용매

반응 조건

온도
0 °C

실험 절차

To a 100 mL flask was added 4-methyl-6-(methyloxy)-3-pyridinamine (850 mg, 6.15 mmol), pyridine (10 mL) and then ethyl chloroformate (0.650 mL, 6.77 mmol) portionwise. The reaction mixture was stirred for 1 h at 0° C. The reaction mixture was then concentrated and partitioned between ammonium chloride and DCM, and the aqueous layer was extracted with DCM (2×). The combined organics layers were washed with brine (1×), eluted through a phase separator then concentrated to afford ethyl [4-methyl-6-(methyloxy)-3-pyridinyl]carbamate (1.223 g, 90% yield).

후처리

  1. concentrationThe reaction mixture was then concentrated
  2. custompartitioned between ammonium chloride and DCM
  3. extractionthe aqueous layer was extracted with DCM (2×)
  4. washThe combined organics layers were washed with brine (1×)
  5. washeluted through a phase separator
  6. concentrationthen concentrated

출처 및 근거

ORD 기록
ord-c3e18235a1ff407ebd7487b7b56283d5
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09187464B2

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