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Triethylamine → HCID 69892953、化合物

HRID 48342
ノート
印刷プレビュー

反応式

HRID 48342 の反応式
[Cl:1][C:2]1[CH:3]=[C:4](/[CH:9]=[CH:10]/[C:11]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=2[N:19]([CH3:30])[C:20]([CH2:22][NH:23]C(=O)C(C)(C)C)=[O:21])=O)[CH:5]=[CH:6][C:7]=1[Cl:8].C(N(CC)CC)C>C(OCC)(=O)C.Cl>[Cl:1][C:2]1[CH:3]=[C:4]([CH:5]=[CH:6][C:7]=1[Cl:8])[CH:9]=[CH:10][C:11]1=[N:23][CH2:22][C:20](=[O:21])[N:19]([CH3:30])[C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][C:13]1=2
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 8471TriethylamineHCID 22742421(E)-N-[[N-[2-[3-(3,4-dichlorophenyl)acryloyl]phenyl]-N-methylcarbamoyl]methyl]pivalamide

生成物 1

HCID 69892953HCID 69892953、化合物収率 68.3%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 8857Ethyl Acetate溶媒

実験手順

65 mg (0.14 mmol) of (E)-N-[[N-[2-[3-(3,4-dichlorophenyl)acryloyl]phenyl]-N-methylcarbamoyl]methyl]pivalamide were dissolved in 5 ml of ethyl acetate saturated with hydrogen chloride and were stirred at room temperature for 30 minutes. The solvent was removed by evaporation and the residue dissolved in 5 ml of methanol and 40 mg (0.04 mmol) of triethylamine added. After 2 hours at room temperature the solvent was removed by evaporation and the residue chromatographed on silica gel using ethyl acetate/petrol 2:1 for the elution. There was obtained 33 mg of (E)-5-(3,4-dichlorostyryl)-1,3-dihydro-1-methyl-2H-benzo-1,4-diazepin-2-one as a pale yellow foam. MS: m/e 344.9 [M+H]+.

後処理

  1. customThe solvent was removed by evaporation
  2. dissolutionthe residue dissolved in 5 ml of methanol
  3. customAfter 2 hours at room temperature the solvent was removed by evaporation
  4. customthe residue chromatographed on silica gel
  5. washfor the elution

出典と根拠

ORDレコード
ord-a1987d87efc2427fb6f8b133fffdbeae
出典データセット
uspto-grants-2004_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06703387B2

反応ノート

読み込み中…

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