(Chlorothio)formyl chloride → 5-(4-Benzyloxyphenyl)-[1,3,4]oxathiazol-2-one

HRID 453104

反応式

HRID 453104 の反応式
[CH2:1]([O:8][C:9]1[CH:17]=[CH:16][C:12]([C:13]([NH2:15])=[O:14])=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl[C:19]([S:21]Cl)=[O:20]>C1(C)C=CC=CC=1>[CH2:1]([O:8][C:9]1[CH:10]=[CH:11][C:12]([C:13]2[O:14][C:19](=[O:20])[S:21][N:15]=2)=[CH:16][CH:17]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 75990(Chlorothio)formyl chlorideHCID 27264314-Benzyloxybenzamide

生成物 1

HCID 595495255-(4-Benzyloxyphenyl)-[1,3,4]oxathiazol-2-one

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
90 °C

実験手順

To a solution of 4-benzyloxybenzamide (0.25 g, 1.10 mmol) in toluene (15 ml) was added chlorocarbonylsulfenyl chloride (0.18 ml, 2.20 mmol) and the resulting reaction mixture was refluxed at 90° C. overnight. After the completion of the reaction (TLC monitoring), the mixture was concentrated, added diethyl ether and washed twice with water, twice with 5% NaHCO3, again with water, and was then dried (Na2SO4), concentrated under vacuum to give the product (crude yield 0.310 g, 98%) that was used as such for the next step.

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 twice with water, twice with 5% NaHCO3, again with water
  6. dry with materialwas then dried (Na2SO4)
  7. concentrationconcentrated under vacuum
  8. customto give the product (crude yield 0.310 g, 98%) that

出典と根拠

ORDレコード
ord-c25d00487cf4471eb6576890df02807b
出典データセット
uspto-grants-2013_07
特許番号
US08492414B2

関連ノート

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