Pyridine → 3-Ethyl-3-(4-iodobenzoyloxymethyl) oxetane

HRID 345362

반응식

HRID 345362 반응식
[I:1][C:2]1[CH:10]=[CH:9][C:5]([C:6](Cl)=[O:7])=[CH:4][CH:3]=1.[CH2:11]([C:13]1([CH2:17][OH:18])[CH2:16][O:15][CH2:14]1)[CH3:12].N1C=CC=CC=1>CCOCC>[CH2:11]([C:13]1([CH2:17][O:18][C:6](=[O:7])[C:5]2[CH:9]=[CH:10][C:2]([I:1])=[CH:3][CH:4]=2)[CH2:16][O:15][CH2:14]1)[CH3:12]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 743734-Iodobenzoyl chlorideHCID 76444Oxt-101

생성물 1

HCID 150219453-Ethyl-3-(4-iodobenzoyloxymethyl) oxetane

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

A solution of 4-iodobenzoyl chloride (11.5 gms) in dry ether (50 ml) was added to a stirred solution of 3-ethyl-3-hydroxymethyloxetane (5 gms) and pyridine (3.5 mls) in ether (100 ml) at 0° C. The resulting mixture was allowed to warm to room temperature and stirred for 24 hours. After this time the mixture was washed with water and brine. The organic extracts were dried over anhydrous magnesium sulphate and then evaporated in vacuo. The residue was purified by column chromatography on silica (preeluted with 1% triethylamine in hexane) and eluted with 5% ethyl acetate in hexane. 3-Ethyl-3-(4-iodobenzoyloxymethyl) oxetane was obtained as a colourless oil (8.1 gms).

후처리

  1. washAfter this time the mixture was washed with water and brine
  2. dry with materialThe organic extracts were dried over anhydrous magnesium sulphate
  3. customevaporated in vacuo
  4. customThe residue was purified by column chromatography on silica (preeluted with 1% triethylamine in hexane)
  5. washeluted with 5% ethyl acetate in hexane

출처 및 근거

ORD 기록
ord-93ea95f9c08042d68ed4424179bbfdb1
출처 데이터셋
uspto-grants-1991_10
특허 번호
US05057508

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