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Iodine → HCID 68454768, 화합물

HRID 2358415
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HRID 2358415 반응식
[I:1]I.[C:3]([O:7][C:8](=[O:20])[NH:9][CH2:10][C:11]1[CH:16]=[CH:15][C:14]([NH2:17])=[CH:13][C:12]=1[O:18][CH3:19])([CH3:6])([CH3:5])[CH3:4]>C(Cl)Cl>[C:3]([O:7][C:8](=[O:20])[NH:9][CH2:10][C:11]1[CH:16]=[C:15]([I:1])[C:14]([NH2:17])=[CH:13][C:12]=1[O:18][CH3:19])([CH3:6])([CH3:5])[CH3:4]
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참가 물질

4

반응물 2

HCID 807IodineHCID 68453750HCID 68453750, 화합물

생성물 1

HCID 68454768HCID 68454768, 화합물수율 47%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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온도
0 °C

실험 절차

To a suspension of iodine and AgNO2 in methylene chloride was added a solution of (4-amino-2-methoxy-benzyl)-carbamic acid tert-butyl ester (1.3 g, 5.15 mmol) in methylene chloride at 0° C., and the mixture was stirred for 30 min at 0° C. and more stirred for 30 min at ambient temperature. The reaction was quenched with Na2S2O3. The reaction solution was extracted with methylenechloride, washed with water and brine, dried over anhyd. MgSO4, filtered and concentrated under reduced pressure. The obtained liquid was column-chromatographed (hexane/ethylacetate=2/1) to yield (4-amino-5-iodo-2-methoxy-benzyl)-carbamic acid tert-butyl ester (925 mg, 47%).

후처리

  1. stirringmore stirred for 30 min at ambient temperature
  2. customThe reaction was quenched with Na2S2O3
  3. extractionThe reaction solution was extracted with methylenechloride
  4. washwashed with water and brine
  5. customdried over anhyd
  6. filtrationMgSO4, filtered
  7. concentrationconcentrated under reduced pressure
  8. customThe obtained liquid was column-chromatographed (hexane/ethylacetate=2/1)

출처 및 근거

ORD 기록
ord-4ef023ab31ba43bdb6858b0403e399e7
출처 데이터셋
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07763657B2

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