2-(3-Chloropropyl)-1,3-dioxolane → HCID 53647093、化合物

HRID 355999ノート

反応式

HRID 355999 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 53647093HCID 53647093、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-113df8cd62af48768960ecf8d33604fc
出典データセット
uspto-grants-1998_11
特許番号
US05834493

反応ノート

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