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1,3-Dichloroacetone → 2-(3,4-Bis(benzyloxy)phenyl)-4-chloromethyloxazole

HRID 475554
ノート
印刷プレビュー

反応式

HRID 475554 の反応式
[CH2:1]([O:8][C:9]1[CH:10]=[C:11]([CH:15]=[CH:16][C:17]=1[O:18][CH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[C:12]([NH2:14])=[O:13])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Cl:26][CH2:27][C:28](=O)[CH2:29]Cl>C(O)CC>[CH2:1]([O:8][C:9]1[CH:10]=[C:11]([C:12]2[O:13][CH:29]=[C:28]([CH2:27][Cl:26])[N:14]=2)[CH:15]=[CH:16][C:17]=1[O:18][CH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 107931,3-DichloroacetoneHCID 404187363,4-Bis(benzyloxy)benzamide

生成物 1

HCID 689816632-(3,4-Bis(benzyloxy)phenyl)-4-chloromethyloxazole

試薬・触媒・溶媒 1

HCID 10311-Propanol溶媒

実験手順

A 37.9 g quantity of 3,4-dibenzyloxybenzamide and 28.8 g of 1,3-dichloro-2-propanone were suspended in 500 ml of propanol, and the suspension was heated and refluxed for 3 days. After cooling, the reaction mixture was concentrated to half its original volume under reduced pressure and 300 ml of diisopropyl ether was added. The precipitated crystals were collected by filtration and recrystallized from acetone-methanol-diisopropyl ether. The obtained crystals were dried under reduced pressure to give 20.1 g of colorless powdery 2-(3,4-bis(benzyloxy)phenyl)-4-chloromethyloxazole.

後処理

  1. temperaturethe suspension was heated
  2. temperaturerefluxed for 3 days
  3. temperatureAfter cooling
  4. concentrationthe reaction mixture was concentrated to half its original volume under reduced pressure and 300 ml of diisopropyl ether
  5. additionwas added
  6. filtrationThe precipitated crystals were collected by filtration
  7. customrecrystallized from acetone-methanol-diisopropyl ether
  8. customThe obtained crystals were dried under reduced pressure

出典と根拠

ORDレコード
ord-459b2b5435984085af6de8be3a9e496d
出典データセット
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08637559B2

反応ノート

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