HCID 18353297、化合物 → Methyl 2-(m-methylbenzylthio)-5-trifluoromethylbenzoate

HRID 978087ノート

反応式

HRID 978087 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([CH:20]=[CH:21][CH:22]=1)[CH2:5][S:6][C:7]1[CH:15]=[CH:14][C:13]([C:16]([F:19])([F:18])[F:17])=[CH:12][C:8]=1[C:9]([OH:11])=[O:10].NO[C:25]1CCCCCC=1>C(OCC)C>[CH3:1][C:2]1[CH:3]=[C:4]([CH:20]=[CH:21][CH:22]=1)[CH2:5][S:6][C:7]1[CH:15]=[CH:14][C:13]([C:16]([F:17])([F:18])[F:19])=[CH:12][C:8]=1[C:9]([O:11][CH3:25])=[O:10]

参加物

4

反応物 2

HCID 18353297HCID 18353297、化合物HCID 202050722-(m-Methylbenzylthio)-5-trifluoromethylbenzoic acid

生成物 1

HCID 13787728Methyl 2-(m-methylbenzylthio)-5-trifluoromethylbenzoate

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

A mixture of 2-(m-methylbenzylthio)-5-trifluoromethylbenzoic acid (1.65 g, 5.06 mmol) and 1-aza-2-methoxy-1-cycloheptene (643 mg, 5.06 mmol) was heated at 80°-85° C. for 18 hours, cooled, diluted with diethyl ether, washed with 1N aqueous sodium hydroxide solution, water, dried (sodium sulfate), and evaporated. The product was crystallized from methanol; yield 885 mg (51%). The 60 MHz NMR spectrum in chloroform-d was in accord with the desired structure.

後処理

  1. temperaturewas heated at 80°-85° C. for 18 hours
  2. temperaturecooled
  3. washwashed with 1N aqueous sodium hydroxide solution, water
  4. dry with materialdried (sodium sulfate)
  5. customevaporated
  6. customThe product was crystallized from methanol

出典と根拠

ORDレコード
ord-a03ea212e42c44d9a79ad93b0a770a3e
出典データセット
uspto-grants-1987_05
特許番号
US04663344

反応ノート

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