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

HRID 17384

反応式

HRID 17384 の反応式
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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3c23cc3f34664b59a15fc35c79f1eae3
出典データセット
uspto-grants-2010_06
特許番号
US07737166B2

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