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Acetic Acid → N-(3-chloropropyl)-6-acetyl-2-benzoxazolinone

HRID 1078851
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인쇄 미리보기

반응식

HRID 1078851 반응식
[Cl:1][CH2:2][CH2:3][CH2:4][N:5]1[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[O:7][C:6]1=[O:14].[C:15](O)(=[O:17])[CH3:16]>>[Cl:1][CH2:2][CH2:3][CH2:4][N:5]1[C:9]2[CH:10]=[CH:11][C:12]([C:15](=[O:17])[CH3:16])=[CH:13][C:8]=2[O:7][C:6]1=[O:14]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 176Acetic AcidHCID 100360722(3H)-Benzoxazolone, 3-(3-chloropropyl)-

생성물 1

HCID 10400030N-(3-chloropropyl)-6-acetyl-2-benzoxazolinone

반응 조건

온도
100 °C

실험 절차

A mixture of N-(3-chloropropyl)-2-benzoxazolinone (8.5 g, 40 mmol), polyphosphoric acid (100 g), and acetic acid (2.4 g, 2.3 ml, 40 mmol), was stirred and heated at 100° C. for 2 hours. The hot solution was poured into ice-water to deposit a yellow gum. The mixture was extracted with dichloromethane, and insolubles were filtered. The dichloromethane extract was washed with water, dried (K2CO3), and concentrated to afford 6.4 g of a slightly green solid. This was recrystallized from ethanol (95%) to yield N-(3-chloropropyl)-6-acetyl-2-benzoxazolinone as a brown solid, 3.5 g,

후처리

  1. extraction
The mixture was extracted with dichloromethane, and insolubles
  • filtrationwere filtered
  • extractionThe dichloromethane extract
  • washwas washed with water
  • dry with materialdried (K2CO3)
  • concentrationconcentrated
  • customto afford 6.4 g of a slightly green solid
  • customThis was recrystallized from ethanol (95%)
  • 출처 및 근거

    ORD 기록
    ord-6ffbfdd5e6e24fcdb05d31fe6ecab2e9
    출처 데이터셋
    uspto-grants-1996_08
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US05550130

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