2,4-Dimethoxybenzoic acid → HCID 19040985, 화합물

HRID 2399947노트

반응식

HRID 2399947 반응식
[CH3:1][O:2][C:3]1[CH:11]=[C:10]([O:12][CH3:13])[CH:9]=[CH:8][C:4]=1[C:5]([OH:7])=O.[CH:14]([NH:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)([CH3:16])[CH3:15].OC1C2N=NNC=2C=CC=1.Cl.C(N=C=NCCCN(C)C)C>ClCCl>[CH3:1][O:2][C:3]1[CH:11]=[C:10]([O:12][CH3:13])[CH:9]=[CH:8][C:4]=1[C:5]([N:17]([CH:14]([CH3:16])[CH3:15])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)=[O:7]

참가 물질

6

반응물 4

HCID 70522,4-Dimethoxybenzoic acidHCID 13032N-IsopropylanilineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 178418300HCID 178418300, 화합물

생성물 1

HCID 19040985HCID 19040985, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A stirred solution of 2,4-dimethoxybenzoic acid (4.31 g, 23.7 mmol) in 35 mL of dichloromethane is treated with N-isopropylaniline (3.07 mL, 21.33 mmol), hydroxybenzotriazole (3.2 g, 23.7 mmol), and 1-ethyl-3-[3-(dimethylamino)propyl]-carbodiimide hydrochloride (4.54 g, 23.7 mmol). This solution is stirred at room temperature for 18 hours and the resulting solution is partitioned between ethyl acetate and 1N hydrochloride solution. The organic layer is washed with water, dried over sodium sulfate and concentrated. The resulting material is purified by chromatography on silica gel (150 g) with 40-60% ethyl acetate/hexane as the eluent to afford 2,4-dimethoxy-N-(1-methylethyl)-N-phenylbenzamide as a colorless foam.

후처리

  1. customthe resulting solution is partitioned between ethyl acetate and 1N hydrochloride solution
  2. washThe organic layer is washed with water
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated
  5. customThe resulting material is purified by chromatography on silica gel (150 g) with 40-60% ethyl acetate/hexane as the eluent

출처 및 근거

ORD 기록
ord-2623c8935b6b43a6adb1dd4b8de9f75b
출처 데이터셋
uspto-grants-1995_09
특허 번호
US05451700

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