Pyridine → HCID 178479470, 화합물

HRID 2119024

반응식

HRID 2119024 반응식
[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][C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)(=[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])[C:27]1[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=1

참가 물질

6

반응물 4

HCID 1049PyridineHCID 10868DicyclohexylcarbodiimideHCID 522771Benzyl anthranilateHCID 178479474HCID 178479474, 화합물

생성물 1

HCID 178479470HCID 178479470, 화합물수율 55.3%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Trans-4-guanidinomethylcyclohexanecarboxylic acid hydrochloride (3.0 g, 0.013 mole) (which is prepared by the method as disclosed in Japanese Patent First Publication No. 19694/1977, C.A., 87, 53269x) and benzyl anthranilate (3.4 g, 0.015 mole) are added to pyridine (25 ml), and thereto is added dicyclohexylcarbodiimide (3.1 g, 0.015 mole), and the mixture is stirred at room temperature for 72 hours. After the completion of the reaction, water (10 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 driness. The resulting residue is washed with ethyl acetate (100 ml) and recrystallized from water to give N-(o-benzyloxycarbonylphenyl)-trans-4-guanidinomethylcyclohexanecarboxamide hydrochloride (3.2 g) as white crystals. m.p. 93°-95° C.

후처리

  1. additionis added to the reaction mixture
  2. stirringthe mixture is stirred for 30 minutes
  3. filtrationthe undissolved materials are filtered off
  4. concentrationThe filtrate is concentrated to driness
  5. washThe resulting residue is washed with ethyl acetate (100 ml)
  6. customrecrystallized from water

출처 및 근거

ORD 기록
ord-7b8dfbee549848a09ab367860088d6cc
출처 데이터셋
uspto-grants-1987_07
특허 번호
US04681895

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