3-Benzyloxy-5-(methylsulfonyl)-2-thiophenecarboxylic Acid → 4-Benzyloxy-2-(methylsulfonyl)thiophene

HRID 1953965노트

반응식

HRID 1953965 반응식
[CH2:1]([O:8][C:9]1[CH:13]=[C:12]([S:14]([CH3:17])(=[O:16])=[O:15])[S:11][C:10]=1C(O)=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>N1C2C(=CC=CC=2)C=CC=1>[CH2:1]([O:8][C:9]1[CH:13]=[C:12]([S:14]([CH3:17])(=[O:16])=[O:15])[S:11][CH:10]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

3

반응물 1

HCID 154771003-Benzyloxy-5-(methylsulfonyl)-2-thiophenecarboxylic Acid

생성물 1

HCID 154771014-Benzyloxy-2-(methylsulfonyl)thiophene수율 86%

시약·촉매·용매 1

HCID 7047Quinoline용매

반응 조건

온도
165 °C

실험 절차

A solution of 3-benzyloxy-5-(methylsulfonyl)-2-thiopenecarboxylic acid (13.6 g, 43.6 mmol) in 50 ml quinoline is treated with Cu powder (4.15 g, 65.4 mmol) at room temperature, heated to 165° C. for 15 minutes, cooled to room temperature and filtered. (The filtercake is washed with water.) The combined filtrate is acidified to pH 1 with 6N HCl and filtered. This filtercake is washed with water and dried to afford the title product as a dark grey powder, 10.1 g (86% yield), mp 108-109° C., identified by 1HNMR, 13CNMR and mass spectral analyses.

후처리

  1. temperaturecooled to room temperature
  2. filtrationfiltered
  3. wash(The filtercake is washed with water
  4. filtrationfiltered
  5. washThis filtercake is washed with water
  6. customdried

출처 및 근거

ORD 기록
ord-93b5e80c704445278fcad4cb2e49b352
출처 데이터셋
uspto-grants-2000_09
특허 번호
US06121202

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