Iodylbenzene → HCID 86655984, 화합물

HRID 1188748노트

반응식

HRID 1188748 반응식
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]

참가 물질

5

반응물 3

HCID 101840IodylbenzeneHCID 115197DimethyldioxiraneHCID 67081740HCID 67081740, 화합물

생성물 1

HCID 86655984HCID 86655984, 화합물수율 84%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ce54a8482a2046ae913743c35f2ead7a
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08674101B2

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