Hydrochloric Acid → 4-cyano-7-fluoro-N,5-dimethyl-6-phenyl-N-(2-phenylethyl)-1,3-benzoxazole-2-carboxamide

HRID 17384

반응식

HRID 17384 반응식
C[Al](C)C.[CH3:5][NH:6][CH2:7][CH2:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.[C:15]([C:17]1[C:22]2[N:23]=[C:24]([C:26]([O:28]CC)=O)[O:25][C:21]=2[C:20]([F:31])=[C:19]([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[C:18]=1[CH3:38])#[N:16].Cl>ClCCl>[C:15]([C:17]1[C:22]2[N:23]=[C:24]([C:26]([N:6]([CH3:5])[CH2:7][CH2:8][C:9]3[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=3)=[O:28])[O:25][C:21]=2[C:20]([F:31])=[C:19]([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[C:18]=1[CH3:38])#[N:16]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 11503N-MethylbenzeneethanamineHCID 16682925TrimethylaluminumHCID 51041426Ethyl 4-cyano-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-2-carboxylate

생성물 1

HCID 685850784-cyano-7-fluoro-N,5-dimethyl-6-phenyl-N-(2-phenylethyl)-1,3-benzoxazole-2-carboxamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

Under nitrogen atmosphere, trimethylaluminium (1.03 M n-hexane solution, 1.80 ml, 1.85 mmol) was dropwise added at room temperature to a dichloromethane (3 ml) solution of N-methylphenethylamine (269 μl, 1.85 mmol), and stirred for 25 minutes. Subsequently, a dichloromethane (3 ml) solution of ethyl 4-cyano-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-2-carboxylate (I-111) (300 mg, 925 μl) was dropwise added and stirred for 14.5 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.

후처리

  1. stirringstirred for 14.5 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

출처 및 근거

ORD 기록
ord-3c23cc3f34664b59a15fc35c79f1eae3
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07737166B2

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