Pyridine → HCID 178468799, 화합물

HRID 2119022

반응식

HRID 2119022 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][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]

참가 물질

6

반응물 4

HCID 1049PyridineHCID 6877Ethyl 2-aminobenzoateHCID 10868DicyclohexylcarbodiimideHCID 178479474HCID 178479474, 화합물

생성물 1

HCID 178468799HCID 178468799, 화합물수율 41.9%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e94ce90f3b1545ac9c7615fd226e4cb5
출처 데이터셋
uspto-grants-1987_07
특허 번호
US04681895

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