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Diisopropylethylamine → N-[3-(2-Methylaminoethoxy)-4-methoxyphenyl]-2'-methyl-4'-(5-methyl-1,2,4-oxadiazol-3-yl)biphenyl-4-carboxamide

HRID 2392683
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HRID 2392683 반응식
[CH3:1][N:2](C)[CH2:3][CH2:4][O:5][C:6]1[CH:7]=[C:8]([NH:14][C:15]([C:17]2[CH:22]=[CH:21][C:20]([C:23]3[CH:28]=[CH:27][C:26]([C:29]4[N:33]=[C:32]([CH3:34])[O:31][N:30]=4)=[CH:25][C:24]=3[CH3:35])=[CH:19][CH:18]=2)=[O:16])[CH:9]=[CH:10][C:11]=1[O:12][CH3:13].ClC(OC(Cl)C)=O.C(N(C(C)C)CC)(C)C>ClCCCl>[CH3:1][NH:2][CH2:3][CH2:4][O:5][C:6]1[CH:7]=[C:8]([NH:14][C:15]([C:17]2[CH:18]=[CH:19][C:20]([C:23]3[CH:28]=[CH:27][C:26]([C:29]4[N:33]=[C:32]([CH3:34])[O:31][N:30]=4)=[CH:25][C:24]=3[CH3:35])=[CH:21][CH:22]=2)=[O:16])[CH:9]=[CH:10][C:11]=1[O:12][CH3:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 5213051-Chloroethyl chloroformateHCID 3292447SB 216641

생성물 1

HCID 18672663N-[3-(2-Methylaminoethoxy)-4-methoxyphenyl]-2'-methyl-4'-(5-methyl-1,2,4-oxadiazol-3-yl)biphenyl-4-carboxamide수율 68%

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

A solution of N-[3-(2-dimethylaminoethoxy)-4-methoxyphenyl]-2'-methyl-4'-(5-methyl-1,2,4-oxadiazol-3-yl)biphenyl-4-carboxamide (E1, 0.2 g, 0.41 mmole) in 1,2-dichloroethane (5 ml) was treated at room temperature with 1-chloroethyl chloroformate (0.12 ml, 1.12 mmole) followed by diisopropylethylamine (0.15 ml, 0.86 mmole). The mixture was stirred for 2 hours at room temperature. After removal of solvent in vacuo the residue was treated with methanol (8 ml) and heated under reflux for 30 minutes. The reaction mixture was concentrated in vacuo and the residue treated with saturated aqueous potassium carbonate (10 ml) and extracted with dichloromethane (3×10 ml). The combined organic extracts were dried and concentrated in vacuo. Flash column chromatography on silica gel eluting with 5% MeOH/CH2Cl2 gave the title compound as a light pink solid (0.13 g, 68%) mp 97°-99° C.

후처리

  1. customAfter removal of solvent in vacuo the residue
  2. additionwas treated with methanol (8 ml)
  3. temperatureheated
  4. temperatureunder reflux for 30 minutes
  5. concentrationThe reaction mixture was concentrated in vacuo
  6. additionthe residue treated with saturated aqueous potassium carbonate (10 ml)
  7. extractionextracted with dichloromethane (3×10 ml)
  8. customThe combined organic extracts were dried
  9. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-f3d1e8c08a9f4dc5872255e119ad054f
출처 데이터셋
uspto-grants-1998_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05801170

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