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

HRID 1953965ノート

反応式

HRID 1953965 の反応式
[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

参加物

3

反応物 1

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

生成物 1

HCID 154771014-Benzyloxy-2-(methylsulfonyl)thiophene収率 86%

試薬・触媒・溶媒 1

HCID 7047Quinoline溶媒

反応条件

温度
165 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-93b5e80c704445278fcad4cb2e49b352
出典データセット
uspto-grants-2000_09
特許番号
US06121202

反応ノート

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