Hydrochloric Acid → N5-(7-Methoxyquinolin-4-yl)pyrimidine-2,5-diamine

HRID 1013699노트

반응식

HRID 1013699 반응식
[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7]([NH:13][C:14]3[CH:15]=[N:16][C:17]([NH:20]C(=O)C4C=CC=CC=4)=[N:18][CH:19]=3)=[CH:8][CH:9]=[N:10]2)=[CH:5][CH:4]=1.Cl>CO>[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7]([NH:13][C:14]3[CH:15]=[N:16][C:17]([NH2:20])=[N:18][CH:19]=3)=[CH:8][CH:9]=[N:10]2)=[CH:5][CH:4]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 67316087N-(5-(7-Methoxyquinolin-4-ylamino)pyrimidin-2-yl)benzamide

생성물 1

HCID 59427342N5-(7-Methoxyquinolin-4-yl)pyrimidine-2,5-diamine

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
80 °C

실험 절차

In 25 mL sealed tube, N-(5-(7-methoxyquinolin-4-ylamino)pyrimidin-2-yl)benzamide (400 mg, 1077 μmol) was added into 6 ml of MeOH followed by addition of 2 mL of HCl (conc.). The reaction was heated at 80° C. After 1.5 h the reaction mixture based on LCMS showed full conversion to desired product [M+H]++1=269 @ 0.8 min—protonated form. The reaction was cooled to 0° C., 50 mL of CH2Cl2 was added, and the mixture was neutralized with 6N NaOH. Solid precipitated out of the solution in the aqueous layer. The whole mixture was concentrated under reduced pressure. The solid was filtered off with an aid of water to yield a sticky solid. The solid was transferred into a flask with an aid of MeOH. The solvent was evaporated under reduced pressure to afford N5-(7-methoxyquinolin-4-yl)pyrimidine-2,5-diamine as a gray solid.

후처리

  1. customIn 25 mL sealed tube

출처 및 근거

ORD 기록
ord-0587f7b13be3432f8b849aef4bd87448
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07981891B2

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