Triethylamine → HCID 13478095、化合物

HRID 280095

反応式

HRID 280095 の反応式
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

参加物

5

反応物 3

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

生成物 1

HCID 13478095HCID 13478095、化合物

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-08454f3608f04742afd7aee3d64b3985
出典データセット
uspto-grants-1986_05
特許番号
US04588725

関連ノート

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