Benzene → 5-Acetoxy-2-(3-methoxymethoxypropyl)-4,6,7-trimethyl-1,3-benzoxathiole

HRID 2308877노트

반응식

HRID 2308877 반응식
[OH:1][C:2]1[C:3]([CH3:20])=[C:4]([CH3:19])[C:5]2[O:9][CH:8]([CH2:10][CH2:11][CH2:12][O:13][CH2:14][O:15][CH3:16])[S:7][C:6]=2[C:17]=1[CH3:18].[C:21](OC(=O)C)(=[O:23])[CH3:22].C1C=CC=CC=1>N1C=CC=CC=1>[C:21]([O:1][C:2]1[C:3]([CH3:20])=[C:4]([CH3:19])[C:5]2[O:9][CH:8]([CH2:10][CH2:11][CH2:12][O:13][CH2:14][O:15][CH3:16])[S:7][C:6]=2[C:17]=1[CH3:18])(=[O:23])[CH3:22]

참가 물질

5

반응물 3

HCID 241BenzeneHCID 7918Acetic AnhydrideHCID 148021895-Hydroxy-2-(3-methoxymethoxypropyl)-4,6,7-trimethyl-1,3-benzoxathiole

생성물 1

HCID 148021905-Acetoxy-2-(3-methoxymethoxypropyl)-4,6,7-trimethyl-1,3-benzoxathiole

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

100 mg of 5-hydroxy-2-(3-methoxymethoxypropyl)-4,6,7-trimethyl-1,3-benzoxathiole (prepared as described in Example 83) were dissolved in 1 ml of pyridine, and 50 mg of acetic anhydride were added. The reaction mixture was allowed to react for 20 hours at room temperature. Benzene was then added to the reaction mixture, and the benzene solution was washed with water and then dried over anhydrous sodium sulfate. The benzene was distilled off under reduced pressure. The resulting residue was subjected to silica gel column chromatography. The title compound was obtained from the fraction eluted with a 20:1 by volume mixture of benzene and ethyl acetate.

후처리

  1. customto react for 20 hours at room temperature
  2. washthe benzene solution was washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationThe benzene was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-d6ade16802ec4b11ab42ee4907a6d1e6
출처 데이터셋
uspto-grants-1987_09
특허 번호
US04691027

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