Pyridine → HCID 178468799、化合物

HRID 2119022

反応式

HRID 2119022 の反応式
[ClH:1].[NH:2]([CH2:6][C@H:7]1[CH2:12][CH2:11][C@H:10]([C:13]([OH:15])=O)[CH2:9][CH2:8]1)[C:3]([NH2:5])=[NH:4].[C:16]([O:25][CH2:26][CH3:27])(=[O:24])[C:17]1[C:18](=[CH:20][CH:21]=[CH:22][CH:23]=1)[NH2:19].N1C=CC=CC=1.C1(N=C=NC2CCCCC2)CCCCC1>O>[ClH:1].[CH2:26]([O:25][C:16]([C:17]1[CH:23]=[CH:22][CH:21]=[CH:20][C:18]=1[NH:19][C:13]([C@H:10]1[CH2:9][CH2:8][C@H:7]([CH2:6][NH:2][C:3]([NH2:5])=[NH:4])[CH2:12][CH2:11]1)=[O:15])=[O:24])[CH3:27]

参加物

6

反応物 4

HCID 1049PyridineHCID 6877Ethyl 2-aminobenzoateHCID 10868DicyclohexylcarbodiimideHCID 178479474HCID 178479474、化合物

生成物 1

HCID 178468799HCID 178468799、化合物収率 41.9%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Trans-4-guanidinomethylcyclohexanecarboxylic acid hydrochloride (10.0 g, 0.042 mole) (which is prepared by the method as disclosed in Japanese Patent First Publication No. 19694/1977, C.A., 87, 53269x) and ethyl anthranilate (10.4 g, 0.063 mole) are added to pyridine (50 ml), and the mixture is stirred for a while, and thereto is added dicyclohexylcarbodiimide (13 g, 0.063 mole), and the mixture is stirred at room temperature for 72 hours. After the completion of the reaction, water (30 ml) is added to the reaction mixture, and the mixture is stirred for 30 minutes, and the undissolved materials are filtered off. The filtrate is concentrated to dryness. The resulting residue is washed with ethyl acetate (300 ml) and recrystallized from water to give the title compound (6.74 g) as white crystals. m.p. 92°-95° C.

後処理

  1. stirringthe mixture is stirred at room temperature for 72 hours
  2. additionis added to the reaction mixture
  3. stirringthe mixture is stirred for 30 minutes
  4. filtrationthe undissolved materials are filtered off
  5. concentrationThe filtrate is concentrated to dryness
  6. washThe resulting residue is washed with ethyl acetate (300 ml)
  7. customrecrystallized from water

出典と根拠

ORDレコード
ord-e94ce90f3b1545ac9c7615fd226e4cb5
出典データセット
uspto-grants-1987_07
特許番号
US04681895

関連ノート

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