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Hydrochloric Acid → tert-Butyl [(4-cyano-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-2-carbonyl)methylamino]acetate

HRID 17493
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HRID 17493 반응식
C[Al](C)C.Cl.[C:6]([O:10][C:11](=[O:15])[CH2:12][NH:13][CH3:14])([CH3:9])([CH3:8])[CH3:7].[C:16]([C:18]1[C:23]2[N:24]=[C:25]([C:27](OCC)=[O:28])[O:26][C:22]=2[C:21]([F:32])=[C:20]([C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)[C:19]=1[CH3:39])#[N:17].Cl>ClCCl>[C:16]([C:18]1[C:23]2[N:24]=[C:25]([C:27]([CH2:14][NH:13][CH2:12][C:11]([O:10][C:6]([CH3:9])([CH3:8])[CH3:7])=[O:15])=[O:28])[O:26][C:22]=2[C:21]([F:32])=[C:20]([C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)[C:19]=1[CH3:39])#[N:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 11252350Sarcosine t-butyl ester hydrochlorideHCID 16682925TrimethylaluminumHCID 51041426Ethyl 4-cyano-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-2-carboxylate

생성물 1

HCID 86630857tert-Butyl [(4-cyano-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-2-carbonyl)methylamino]acetate수율 87.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

Under nitrogen atmosphere, trimethylaluminium (1.03 M n-hexane solution, 4.50 ml, 4.63 mmol) was dropwise added at room temperature to a dichloromethane (6 ml) solution of N-methylglycine tert-butyl ester hydrochloride (840 mg, 4.63 mmol), followed by stirring for 25 hours. Subsequently, a dichloromethane (4 ml) solution of ethyl 4-cyano-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-2-carboxylate (I-111) (500 mg, 1.54 mmol) was dropwise added, followed by stirring for 23 hours. After the reaction, aqueous 1 N hydrochloric acid solution was added to the reaction liquid with cooling with ice, followed by stirring at room temperature, and the reaction liquid was extracted with chloroform. Next, the obtained organic layers were combined, dried over anhydrous magnesium sulfate, filtered, and the filtrate was concentrated under reduced pressure. The resulting residue was suspended and washed in diethyl ether to obtain the entitled compound (569 mg, 87%) as a white solid.

후처리

  1. stirringby stirring for 23 hours
  2. additionwas added to the reaction liquid
  3. temperaturewith cooling with ice
  4. stirringby stirring at room temperature
  5. customthe reaction liquid
  6. extractionwas extracted with chloroform
  7. dry with materialdried over anhydrous magnesium sulfate
  8. filtrationfiltered
  9. concentrationthe filtrate was concentrated under reduced pressure
  10. washwashed in diethyl ether

출처 및 근거

ORD 기록
ord-abec07b406974cb0a332db3ca8eef204
출처 데이터셋
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07737166B2

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