Allyl chloride → [4-(Acryloylmethylamino)phenyl]acetic Acid Methyl Ester

HRID 1097074노트

반응식

HRID 1097074 반응식
[CH3:1][O:2][C:3](=[O:13])[CH2:4][C:5]1[CH:10]=[CH:9][C:8]([NH:11][CH3:12])=[CH:7][CH:6]=1.[CH:14](N(CC)C(C)C)([CH3:16])[CH3:15].C(Cl)C=C.C(=O)(O)[O-:28].[Na+]>C(Cl)Cl>[CH3:1][O:2][C:3](=[O:13])[CH2:4][C:5]1[CH:10]=[CH:9][C:8]([NH:11][CH2:12][C:15](=[O:28])[CH:14]=[CH2:16])=[CH:7][CH:6]=1

참가 물질

6

반응물 4

HCID 7850Allyl chlorideHCID 81531DiisopropylethylamineHCID 516892Sodium BicarbonateHCID 15892780Methyl 2-(4-(methylamino)phenyl)acetate

생성물 1

HCID 66770363[4-(Acryloylmethylamino)phenyl]acetic Acid Methyl Ester

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of methyl(4-methylaminophenyl)acetate (4.00 g, 22.3 mmol) and N,N-diisopropylethylamine (7.78 mL, 44.6 mmol) in DCM (20.0 mL) at 0° C. was slowly added 2-propenyl chloride (2.18 mL, 26.8 mmol). The reaction mixture was stirred at room temperature for 2 h and then saturated aqueous sodium bicarbonate (20.0 mL) was added. This mixture was extracted with DCM (10 mL) and the organic layer was dried over sodium sulfate, filtered and concentrated under reduced pressure to give the title compound, which was used in the next reaction without further purification.

후처리

  1. customat 0° C.
  2. extractionThis mixture was extracted with DCM (10 mL)
  3. dry with materialthe organic layer was dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-2e9913742360498bbec166cd0bd5e362
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08138345B2

반응 노트

불러오는 중…