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

HRID 475554
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HRID 475554 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 10311-Propanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-459b2b5435984085af6de8be3a9e496d
출처 데이터셋
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08637559B2

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