Iodylbenzene → HCID 86655984、化合物

HRID 1188748ノート

反応式

HRID 1188748 の反応式
CC1(C)OO1.[I:6]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)(=[O:8])=[O:7].IC1C=CC([C:22]2[S:23][C:24]3[CH:30]=[C:29]([O:31][CH3:32])[CH:28]=[CH:27][C:25]=3[N:26]=2)=CC=1>ClCCl>[I:6]([C:9]1[CH:14]=[CH:13][C:12]([C:22]2[S:23][C:24]3[CH:30]=[C:29]([O:31][CH3:32])[CH:28]=[CH:27][C:25]=3[N:26]=2)=[CH:11][CH:10]=1)(=[O:8])=[O:7]

参加物

5

反応物 3

HCID 101840IodylbenzeneHCID 115197DimethyldioxiraneHCID 67081740HCID 67081740、化合物

生成物 1

HCID 86655984HCID 86655984、化合物収率 84%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A freshly prepared dimethyldioxirane solution (30 mL), as described above (para. [0035]) for the synthesis of simple iodylbenzene analogs, was added drop wise with stirring to an anhydrous dichloromethane (15 mL) solution of 4 (100 mg, 0.28 mmol) cooled in an ice bath. The resultant suspension was stirred at 0° C. for additional period of 2-3 hours and then at room temperature overnight. The yellow solid that was formed was collected by centrifugation and washed three times with dichloromethane. The residue was dried in vacuum to give 2-(4-iodylphenyl)-6-methoxy-1,3-benzothiazole (7) (95.4 mg, 84%) as a beige solid.

後処理

  1. additionwas added drop wise
  2. temperaturecooled in an ice bath
  3. customat room temperature
  4. customovernight
  5. customThe yellow solid that was formed
  6. customwas collected by centrifugation
  7. washwashed three times with dichloromethane
  8. customThe residue was dried in vacuum

出典と根拠

ORDレコード
ord-ce54a8482a2046ae913743c35f2ead7a
出典データセット
uspto-grants-2014_03
特許番号
US08674101B2

反応ノート

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