3-Aminobenzoic Acid → HCID 178479313、化合物

HRID 378126

反応式

HRID 378126 の反応式
[ClH:1].[C:2](=[NH:12])(OCC)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.C(N(C(C)C)CC)(C)C.[NH2:22][C:23]1[CH:24]=[C:25]([CH:29]=[CH:30][CH:31]=1)[C:26]([OH:28])=[O:27]>O.O1CCOCC1>[ClH:1].[C:26]([C:25]1[CH:24]=[C:23]([NH:22][C:2](=[NH:12])[C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH:31]=[CH:30][CH:29]=1)([OH:28])=[O:27]

参加物

6

反応物 3

HCID 74193-Aminobenzoic AcidHCID 79249Benzenecarboximidic acid, ethyl ester, hydrochloride (1:1)HCID 81531Diisopropylethylamine

生成物 1

HCID 178479313HCID 178479313、化合物収率 15.8%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

To ethyl benzimidate hydrochloride (3 g, 0.016 mole)(Fluka) and (2.1 g, 0.016 mole) diisopropylethylamine in H2O (15 ml) and dioxane (15 ml) was added 3-aminobenzoic acid (2.22 g, 0.016 mole) (Aldrich). The reaction mixture was stirred at room temperature for 4 days. The resulting precipitate was filtered, washed with dioxane/H2O and dried. The precipitate was slurried in H2O and acidified with concentrated HCl. The solvent was removed under vacuum and the residue was slurried in ether. The ether was decanted off and the residue dried under vacuum to yield N-(3-carboxyphenyl)benzamidine hydrochloride (700 mg) as a white solid. MS and NMR were consistent with the desired structure.

後処理

  1. filtrationThe resulting precipitate was filtered
  2. washwashed with dioxane/H2O
  3. customdried
  4. customThe solvent was removed under vacuum
  5. customThe ether was decanted off
  6. customthe residue dried under vacuum

出典と根拠

ORDレコード
ord-20ecb093fda34faba4686369b6b1f19d
出典データセット
uspto-grants-2000_02
特許番号
US06028223

関連ノート

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