Benzoyl chloride → N-(1-Ethoxycyclopropyl)benzenecarboximidic acid

HRID 616976ノート

反応式

HRID 616976 の反応式
C(N(CC)CC)C.[Cl-].[CH2:9]([O:11][C:12]1([NH3+:15])[CH2:14][CH2:13]1)[CH3:10].[C:16](Cl)(=[O:23])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>O1CCCC1>[CH2:9]([O:11][C:12]1([NH:15][C:16](=[O:23])[C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH2:14][CH2:13]1)[CH3:10]

参加物

5

反応物 3

HCID 7412Benzoyl chlorideHCID 8471TriethylamineHCID 20367034HCID 20367034、化合物

生成物 1

HCID 125108N-(1-Ethoxycyclopropyl)benzenecarboximidic acid

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Triethylamine (2.5 g, 25 mmol) is added dropwise at 0° to a solution of 1-ethoxycyclopropylammonium chloride (1.25 g, 9.15 mmol) and benzoyl chloride (1.4 g, 10 mmol) in dry tetrahydrofuran (20 ml). The precipitate is filtered off and the filtrate is evaporated in vacuo yielding a crystalline residue. Sublimation following by recrystallisation from cyclohexane gives N-(1-ethoxycyclopropyl)-benzamide, mp 108°-109° (0.95 g, 51%); NMR (60 MHz): δCDCl 3 = 0.90-1.38 (m, 4H), 1.16 (t, J=7 Hz, 3H), 3.77 (q, J=7 Hz, 2H), 7.0-8.0 (1 m and 1 br. s, total 6H).

後処理

  1. filtrationThe precipitate is filtered off
  2. customthe filtrate is evaporated in vacuo
  3. customyielding a crystalline residue
  4. customSublimation following by recrystallisation from cyclohexane

出典と根拠

ORDレコード
ord-c5bff4d1c3994bdab4a91ce598ed6d0d
出典データセット
uspto-grants-1978_02
特許番号
US04076840

反応ノート

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