Pyridine → HCID 178497648, 화합물

HRID 2119023

반응식

HRID 2119023 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][CH3:26])(=[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].[CH3:26][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]

참가 물질

6

반응물 4

HCID 1049PyridineHCID 8635Methyl AnthranilateHCID 10868DicyclohexylcarbodiimideHCID 178479474HCID 178479474, 화합물

생성물 1

HCID 178497648HCID 178497648, 화합물수율 46.5%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Trans-4-guanidinomethylcyclohexanecarboxylic acid hydrochloride (3 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 methyl anthranilate (2.3 g, 0.015 mole) are added to pyridine (20 ml), and the mixture is stirred for a while, 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 dryness. The resulting residue is washed with ethyl acetate (100 ml) and recrystallized from water to give the title compound (2.23 g) as white crystals. m.p. 118.5°-120.5° 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 (100 ml)
  7. customrecrystallized from water

출처 및 근거

ORD 기록
ord-744d9ce5058b406d8f45319bd435d81a
출처 데이터셋
uspto-grants-1987_07
특허 번호
US04681895

연결된 노트

불러오는 중…