(Chlorothio)formyl chloride → 5-(4-Methoxyphenyl)-1,3,4-oxathiazol-2-one

HRID 453089ノート

反応式

HRID 453089 の反応式
[CH3:1][O:2][C:3]1[CH:11]=[CH:10][C:6]([C:7]([NH2:9])=[O:8])=[CH:5][CH:4]=1.Cl[C:13]([S:15]Cl)=[O:14]>C1(C)C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:11]=[CH:10][C:6]([C:7]2[O:8][C:13](=[O:14])[S:15][N:9]=2)=[CH:5][CH:4]=1

参加物

4

反応物 2

HCID 75990(Chlorothio)formyl chlorideHCID 769594-Methoxybenzamide

生成物 1

HCID 8194565-(4-Methoxyphenyl)-1,3,4-oxathiazol-2-one

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
80 °C

実験手順

To a solution of 4-methoxybenzamide (0.30 g, 1.10 mmol) in toluene (10 ml) was added chlorocarbonylsulfenyl chloride (0.80 ml, 9.92 mmol). The resulting reaction mixture was refluxed at 80° C. for 3 h. After the completion of the reaction (TLC monitoring), the mixture was concentrated, added diethyl ether and washed with twice with water, twice with 5% NaHCO3, again with water, and was dried (Na2SO4), concentrated under vacuum to give the product (crude yield 0.475 g) that was carried forward to the next step without further purification.

後処理

  1. customThe resulting reaction mixture
  2. customAfter the completion of the reaction (TLC monitoring)
  3. concentrationthe mixture was concentrated
  4. additionadded diethyl ether
  5. washwashed with twice with water
  6. dry with materialtwice with 5% NaHCO3, again with water, and was dried (Na2SO4)
  7. concentrationconcentrated under vacuum
  8. customto give the product (crude yield 0.475 g) that
  9. customwas carried forward to the next step without further purification

出典と根拠

ORDレコード
ord-848742b7949449a7b4dacf7d6e2bf053
出典データセット
uspto-grants-2013_07
特許番号
US08492414B2

反応ノート

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