Dichloromethane → 3-Ethoxy-4-methoxybenzoyl chloride

HRID 238060노트

반응식

HRID 238060 반응식
[CH2:1]([O:3][C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][C:12]=1[O:13][CH3:14])[C:7](O)=[O:8])[CH3:2].C(Cl)[Cl:16].C(Cl)(=O)C(Cl)=O>CN(C=O)C.C1C=CC=CC=1>[CH2:1]([O:3][C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][C:12]=1[O:13][CH3:14])[C:7]([Cl:16])=[O:8])[CH3:2]

참가 물질

6

반응물 3

HCID 6344DichloromethaneHCID 65578Oxalyl chlorideHCID 28229573-Ethoxy-4-methoxybenzoic acid

생성물 1

HCID 450812503-Ethoxy-4-methoxybenzoyl chloride

시약·촉매·용매 2

HCID 6228Dimethylformamide촉매HCID 241Benzene용매

실험 절차

3-ethoxy-4-methoxybenzoic acid (5 g, 25.5 mmol) was added to a solution of CH2Cl2 (40 mL) and benzene (20 mL) in a flame-dried 150 mL round bottom flask. Anhydrous DMF (9 drops) was added and the solution was cooled on ice. Oxalyl chloride (11 mL, 128 mmol) was added dropwise, and the reaction was then allowed to warm to RT. The reaction was stirred at RT for 90 minutes, then concentrated in vacuo yield an off-white solid. The solid was placed on a high-vacuum line for 2 hours, and then taken onto the next step without further characterization.

후처리

  1. temperaturethe solution was cooled on ice
  2. concentrationconcentrated in vacuo
  3. customyield an off-white solid
  4. waitThe solid was placed on a high-vacuum line for 2 hours

출처 및 근거

ORD 기록
ord-1f03044187f647448e95fefc29def7e7
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08642604B2

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