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Triethylamine → 5-Chloro-2,6-dimethyl-4-{2-[4-(2-ethoxyethyl)-2-methylphenoxy]ethylamino}pyrimidine

HRID 231111
ノート
印刷プレビュー

反応式

HRID 231111 の反応式
C(N(CC)CC)C.[CH2:8]([O:10][CH2:11][CH2:12][C:13]1[CH:22]=[CH:21][C:16]([O:17][CH2:18][CH2:19][NH2:20])=[C:15]([CH3:23])[CH:14]=1)[CH3:9].Cl[C:25]1[C:30]([Cl:31])=[C:29]([CH3:32])[N:28]=[C:27]([CH3:33])[N:26]=1>C1(C)C=CC=CC=1>[Cl:31][C:30]1[C:25]([NH:20][CH2:19][CH2:18][O:17][C:16]2[CH:21]=[CH:22][C:13]([CH2:12][CH2:11][O:10][CH2:8][CH3:9])=[CH:14][C:15]=2[CH3:23])=[N:26][C:27]([CH3:33])=[N:28][C:29]=1[CH3:32]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 139099682-[4-(2-Ethoxyethyl)-2-methylphenoxy]ethan-1-amineHCID 156261074,5-Dichloro-2,6-dimethylpyrimidine

生成物 1

HCID 139099835-Chloro-2,6-dimethyl-4-{2-[4-(2-ethoxyethyl)-2-methylphenoxy]ethylamino}pyrimidine収率 55.8%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

1.0 g of triethylamine and 2.2 g of 2-[4-(2-ethoxyethyl)-2-methylphenoxy]ethylamine were added to 1.8 g of 4,5-dichloro-2,6-dimethylpyrimidine dissolved in 50 ml of toluene. The mixture was heated under reflux, whilst stirring, for 5 hours. At the end of this time, the reaction product was washed with water and dried over anhydrous sodium sulfate. Toluene was then removed by distillation under reduced pressure, and the oily product obtained was subjected to column chromatography (Wakogel C-200, eluted with a 2:1 by volume mixture of toluene and etyl acetate) to isolate the product. The crystals obtained were recrystallized from hexane, to give 2.0 g of the title compound as colorless granular crystals melting at 61°-63° C.

後処理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux
  3. washAt the end of this time, the reaction product was washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. customToluene was then removed by distillation under reduced pressure
  6. customthe oily product obtained
  7. washeluted with a 2:1 by volume mixture of toluene and etyl acetate)
  8. customto isolate the product
  9. customThe crystals obtained
  10. customwere recrystallized from hexane

出典と根拠

ORDレコード
ord-a171694621ec4fe1b4585c73f7e67502
出典データセット
uspto-grants-1989_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04845097

反応ノート

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