Carbon Tetrachloride → HCID 21848394, 화합물

HRID 618769노트

반응식

HRID 618769 반응식
[CH2:1]([O:3][C:4]([CH2:6][NH:7][C:8](=[O:19])[CH2:9][O:10][C:11]1[CH:16]=[CH:15][C:14]([CH2:17]O)=[CH:13][CH:12]=1)=[O:5])[CH3:2].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Cl)(Cl)(Cl)[Cl:40]>C(Cl)Cl>[CH2:1]([O:3][C:4]([CH2:6][NH:7][C:8](=[O:19])[CH2:9][O:10][C:11]1[CH:16]=[CH:15][C:14]([CH2:17][Cl:40])=[CH:13][CH:12]=1)=[O:5])[CH3:2]

참가 물질

5

반응물 3

HCID 5943Carbon TetrachlorideHCID 11776TriphenylphosphineHCID 21848389N-(ethoxycarbonylmethyl)-2-(4-hydroxymethylphenoxy)acetamide

생성물 1

HCID 21848394HCID 21848394, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of N-(ethoxycarbonylmethyl)-2-(4-hydroxymethylphenoxy)acetamide (3.96 g), triphenylphosphine (3.88 g), carbon tetrachloride (10 ml) and methylene chloride (20 ml) was heated at reflux for 1.5 hours. The reaction mixture was evaporated under reduced pressure, and ethyl acetate was added to the residue. After removal of the insolubles by filtration, the filtrate was chromatographed on silica gel column (eluent; ethyl acetate), and the desired fractions were collected and recrystallized from ethyl acetate/ether to give N-(ethoxycarbonylmethyl)-2-(4-chloromethylphenoxy)acetamide (2.8 g).

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 1.5 hours
  3. customThe reaction mixture was evaporated under reduced pressure, and ethyl acetate
  4. additionwas added to the residue
  5. customAfter removal of the insolubles
  6. filtrationby filtration
  7. customthe filtrate was chromatographed on silica gel column (eluent; ethyl acetate)
  8. customthe desired fractions were collected
  9. customrecrystallized from ethyl acetate/ether

출처 및 근거

ORD 기록
ord-d13e9cef9e0f4d6a8e826a9844b19566
출처 데이터셋
uspto-grants-1999_09
특허 번호
US05955505

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