Triethylamine → 4-{N-ethyl-N-[2-(2-methylphenoxy)ethyl]amino}-quinazoline

HRID 1659540

반응식

HRID 1659540 반응식
Cl[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]=[CH:4][N:3]=1.[CH2:12]([NH:14][CH2:15][CH2:16][O:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=1[CH3:24])[CH3:13].C(N(CC)CC)C>C1(C)C=CC=CC=1>[CH2:12]([N:14]([C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]=[CH:4][N:3]=1)[CH2:15][CH2:16][O:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=1[CH3:24])[CH3:13]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 788644-ChloroquinazolineHCID 12797560N-Ethyl-2-(2-methylphenoxy)ethanamine

생성물 1

HCID 127975614-{N-ethyl-N-[2-(2-methylphenoxy)ethyl]amino}-quinazoline수율 54.2%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To a solution of 2.5 g (0.015 mole) of 4-chloroquinazoline in toluene were added 2.7 g (0.015 mole) of N-ethyl-2-(2-methylphenoxy)ethylamine and 1.5 g (0.015 mole) of triethylamine. The mixture was then refluxed, with stirring, for 5.5 hours. After completion of the reaction, the toluene was removed from the reaction mixture by evaporation under reduced pressure. Water was then added to the residue and the mixture was extracted with chloroform and the extract was dried. The chloroform was removed by evaporation and the crystals which separated out were recrystallized from isopropanol, giving 2.5 g (54%) of the desired Compound No. 2, in the form of colourless prisms melting at 85°-87° C.

후처리

  1. temperatureThe mixture was then refluxed
  2. customAfter completion of the reaction
  3. customthe toluene was removed from the reaction mixture by evaporation under reduced pressure
  4. additionWater was then added to the residue
  5. extractionthe mixture was extracted with chloroform
  6. customthe extract was dried
  7. customThe chloroform was removed by evaporation
  8. customthe crystals which separated out
  9. customwere recrystallized from isopropanol

출처 및 근거

ORD 기록
ord-3b6a51e5a21b4f02b5225e21ff2b1bf1
출처 데이터셋
uspto-grants-1981_12
특허 번호
US04304778

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