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Acetonitrile → HCID 68456140, 화합물

HRID 2358420
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HRID 2358420 반응식
Cl.[NH2:2][C:3]1[CH:10]=[CH:9][C:6]([CH2:7][NH2:8])=[CH:5][C:4]=1[F:11].C1([O:18][C:19](=O)[NH:20][CH2:21][C:22]2[CH:27]=[CH:26][C:25]([C:28]([CH3:31])([CH3:30])[CH3:29])=[CH:24][CH:23]=2)C=CC=CC=1.C(#N)C>C(N(CC)CC)C>[NH2:2][C:3]1[CH:10]=[CH:9][C:6]([CH2:7][NH:8][C:19]([NH:20][CH2:21][C:22]2[CH:27]=[CH:26][C:25]([C:28]([CH3:31])([CH3:30])[CH3:29])=[CH:24][CH:23]=2)=[O:18])=[CH:5][C:4]=1[F:11]
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참가 물질

5

반응물 3

HCID 6342AcetonitrileHCID 11708154HCID 11708154, 화합물HCID 59389711Phenyl [(4-tert-butylphenyl)methyl]carbamate

생성물 1

HCID 68456140HCID 68456140, 화합물

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

To the 50 ml of round bottom flask were put 4-amino-3-fluorobenzylamine hydrochloride (0.46 g, 3.28 mmol) and 4-t-butylbenzylcarbamic acid phenyl ester (1.1 eq, 1.02 g). And to this mixture was poured 20 ml acetonitrile and added triethylamine (excess, 0.5 ml) and refluxed 12 hours. After confirming the completion of the reaction with TLC, the reaction mixture was extracted with ethylacetate, washed with 1N HCl solution. And the combined organic layer was dried over MgSO4, filtered and concentrated under reduced pressure. The obtained liquid was column-chromatographed (n-hexane/ethyl acetate=1/1).

후처리

  1. customTo the 50 ml of round bottom flask were put
  2. temperaturerefluxed 12 hours
  3. customthe completion of the reaction with TLC
  4. extractionthe reaction mixture was extracted with ethylacetate
  5. washwashed with 1N HCl solution
  6. dry with materialAnd the combined organic layer was dried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure
  9. customThe obtained liquid was column-chromatographed (n-hexane/ethyl acetate=1/1)

출처 및 근거

ORD 기록
ord-c0ce132ec31b427c8a77426ccd0cc720
출처 데이터셋
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07763657B2

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