Triethylamine → HCID 13478095, 화합물

HRID 280095노트

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HRID 280095 반응식
Cl[C:2]1[N:11]=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.[F:12][C:13]1[CH:18]=[CH:17][C:16]([C:19]2([CH2:24][CH2:25][CH2:26][N:27]3[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]3)OCC[O:20]2)=[CH:15][CH:14]=1.C(N(CC)CC)C>C(O)(C)C>[N:3]1[C:4]2[C:9](=[CH:8][CH:7]=[CH:6][CH:5]=2)[CH:10]=[N:11][C:2]=1[N:30]1[CH2:29][CH2:28][N:27]([CH2:26][CH2:25][CH2:24][C:19]([C:16]2[CH:15]=[CH:14][C:13]([F:12])=[CH:18][CH:17]=2)=[O:20])[CH2:32][CH2:31]1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 740542-ChloroquinazolineHCID 27831211-(3-(2-(4-Fluorophenyl)-1,3-dioxolan-2-yl)propyl)piperazine

생성물 1

HCID 13478095HCID 13478095, 화합물

시약·촉매·용매 1

HCID 3776Isopropanol용매

반응 조건

온도
80 °C

실험 절차

2.25 g 2-Chloroquinazoline, 4.2 g 1-(3-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]-propyl)piperazine and 2 ml triethylamine in 8 ml isopropanol are stirred and heated 21/2 hours at 80° C. The solvent is then evaporated in vacuo and the residue is taken up in hexane. The hexane solution is treated with charcoal, filtered and concentrated whereby the ketal of the title compound crystallizes out. The resulting precipitate is dissolved in 40 ml aqueous 1N hydrochloric acid. After 1 hour the acidic solution is made alkaline with aqueous ammonia. The resulting precipitate is filtered off and recrystallized from ethyl acetate to give the title compound, m.p. 129°-131° C.

후처리

  1. customThe solvent is then evaporated in vacuo
  2. additionThe hexane solution is treated with charcoal
  3. filtrationfiltered
  4. concentrationconcentrated whereby the ketal of the title compound
  5. customcrystallizes out
  6. dissolutionThe resulting precipitate is dissolved in 40 ml aqueous 1N hydrochloric acid
  7. filtrationThe resulting precipitate is filtered off
  8. customrecrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-08454f3608f04742afd7aee3d64b3985
출처 데이터셋
uspto-grants-1986_05
특허 번호
US04588725

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