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Iodine chloride → 1-Iodo-4-isopropyl-2-methoxy-5-(toluene-4-sulfonyl)-benzene

HRID 38394
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반응식

HRID 38394 반응식
[CH:1]([C:4]1[CH:9]=[C:8]([O:10][CH3:11])[CH:7]=[CH:6][C:5]=1[S:12]([C:15]1[CH:20]=[CH:19][C:18]([CH3:21])=[CH:17][CH:16]=1)(=[O:14])=[O:13])([CH3:3])[CH3:2].[I:22]Cl.C([O-])(O)=O.[Na+]>CC(O)=O.O>[I:22][C:7]1[CH:6]=[C:5]([S:12]([C:15]2[CH:16]=[CH:17][C:18]([CH3:21])=[CH:19][CH:20]=2)(=[O:13])=[O:14])[C:4]([CH:1]([CH3:3])[CH3:2])=[CH:9][C:8]=1[O:10][CH3:11]
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참가 물질

6

반응물 3

HCID 24640Iodine chlorideHCID 516892Sodium BicarbonateHCID 670535032-Isopropyl-4-methoxy-1-(toluene-4-sulfonyl)-benzene

생성물 1

HCID 670534521-Iodo-4-isopropyl-2-methoxy-5-(toluene-4-sulfonyl)-benzene수율 91.8%

시약·촉매·용매 2

HCID 176Acetic Acid용매2회
HCID 962
Water
용매

실험 절차

To a solution of 2-Isopropyl-4-methoxy-1-(toluene-4-sulfonyl)-benzene (10 g, 31.25 mmol) in HOAc (10 ml) was added a solution of ICl (9.6 g, 59.26 mmol) in HOAc (10 ml) and H2O (5 ml). The reaction mixture was stirred at room temperature for 16 hrs and basified by saturated NaHCO3 solution. The aqueous solution was extracted into EtOAc which was washed with water, brine, dried over Na2SO4, filtered and concentrated in vacuo to give 1-Iodo-4-isopropyl-2-methoxy-5-(toluene-4-sulfonyl)-benzene (12.35 g, 89%).

후처리

  1. extractionThe aqueous solution was extracted into EtOAc which
  2. washwas washed with water, brine
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-bf078cc3500549939cc948b0ca729321
출처 데이터셋
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08524725B2

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