Triethylamine → methyl 4-[N-[2-(3-cyanophenoxy)ethyl)carbamoyl]benzoate

HRID 747662

反応式

HRID 747662 の反応式
Br.[NH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:7]=[C:8]([CH:11]=[CH:12][CH:13]=1)[C:9]#[N:10].C(N(CC)CC)C.[Cl-].[C:22]([O:33][CH3:34])(=[O:32])[C:23]1[CH:31]=[CH:30][C:26]([C:27]([O-])=[O:28])=[CH:25][CH:24]=1>CN(C)C=O.Cl>[C:9]([C:8]1[CH:7]=[C:6]([CH:13]=[CH:12][CH:11]=1)[O:5][CH2:4][CH2:3][NH:2][C:27]([C:26]1[CH:30]=[CH:31][C:23]([C:22]([O:33][CH3:34])=[O:32])=[CH:24][CH:25]=1)=[O:28])#[N:10]

参加物

6

反応物 3

HCID 8471TriethylamineHCID 177887733-(2-Aminoethoxy)benzonitrile hydrobromideHCID 22493623Monomethyl terephthalate chloride

生成物 1

HCID 68830761methyl 4-[N-[2-(3-cyanophenoxy)ethyl)carbamoyl]benzoate

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 6228Dimethylformamide溶媒

実験手順

1.50 g (6.2 mmol) of 3-(2-aminoethoxy)benzonitrile hydrobromide and 3 ml of triethylamine were stirred in 15 ml of dimethylformamide under cooling with ice. 1.23 g (6.2 mmol) of monomethyl terephthalate chloride was slowly added thereto, and they were stirred for 3 hours. The temperature was elevated to the room temperature, and the reaction liquid was diluted with 1 N hydrochloric acid. After the extraction with ethyl acetate, the organic layer was washed with a saturated aqueous sodium hydrogencarbonate solution and then with saturated aqueous NaCl solution, and then dried over anhydrous magnesium sulfate. The solvent was evaporated to obtain the title compound.

後処理

  1. temperatureunder cooling with ice
  2. customwas elevated to the room temperature
  3. customthe reaction liquid
  4. extractionAfter the extraction with ethyl acetate
  5. washthe organic layer was washed with a saturated aqueous sodium hydrogencarbonate solution
  6. dry with materialwith saturated aqueous NaCl solution, and then dried over anhydrous magnesium sulfate
  7. customThe solvent was evaporated

出典と根拠

ORDレコード
ord-5ebf417277be4a51b4f7be0c7c0f2d75
出典データセット
uspto-grants-2008_07
特許番号
US07396844B1

関連ノート

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