2-(3-Chloropropyl)-1,3-dioxolane → HCID 53647093, 화합물

HRID 355999

반응식

HRID 355999 반응식
[Cl:1][CH2:2][CH2:3][CH2:4][CH:5]1OCCO1.Cl.[C:11]1([O:17][NH2:18])[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1>C1COCC1>[C:11]1([O:17][N:18]=[CH:5][CH2:4][CH2:3][CH2:2][Cl:1])[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1

참가 물질

4

반응물 2

HCID 5520722-(3-Chloropropyl)-1,3-dioxolaneHCID 6365179O-Phenylhydroxylamine hydrochloride

생성물 1

HCID 53647093HCID 53647093, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of 2-(3-chloro-propyl)-[1,3]-dioxolane (5.7 g; 0.038 mol), THF (50 ml) and aqueous acid chloride (1/1) was stirred at room temperature for 24 hours. O-phenyl-hydroxylamine hydrochloride (5 g; 0.034 mol) was then added and the resulting mixture was stirred at room temperature for 48 hours. The reaction mixture was concentrated under vacuum. Then the product was extracted with methylene chloride. The organic extract was dried (Mg SO4) and evaporated under vacuum. After purification by Flash Chromatography on silica gel using as eluent hexane/ethyl acetate (95/5), the desired compound was obtained.

후처리

  1. stirringthe resulting mixture was stirred at room temperature for 48 hours
  2. concentrationThe reaction mixture was concentrated under vacuum
  3. extractionThen the product was extracted with methylene chloride
  4. extractionThe organic extract
  5. dry with materialwas dried (Mg SO4)
  6. customevaporated under vacuum
  7. customAfter purification by Flash Chromatography on silica gel using as eluent hexane/ethyl acetate (95/5)

출처 및 근거

ORD 기록
ord-113df8cd62af48768960ecf8d33604fc
출처 데이터셋
uspto-grants-1998_11
특허 번호
US05834493

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