Hydrochloric Acid → Amino-acetic acid 4-[4-amino-6-(5-chloro-2-methyl-phenyl)-[1,3,5]triazin-2ylamino]-benzyl ester

HRID 1435758

반응식

HRID 1435758 반응식
[NH2:1][C:2]1[N:7]=[C:6]([C:8]2[CH:13]=[C:12]([Cl:14])[CH:11]=[CH:10][C:9]=2[CH3:15])[N:5]=[C:4]([NH:16][C:17]2[CH:35]=[CH:34][C:20]([CH2:21][O:22][C:23](=[O:33])[CH2:24][NH:25]C(OC(C)(C)C)=O)=[CH:19][CH:18]=2)[N:3]=1.ClCCl.Cl.C(OCC)(=O)C>O1CCOCC1>[NH2:1][C:2]1[N:7]=[C:6]([C:8]2[CH:13]=[C:12]([Cl:14])[CH:11]=[CH:10][C:9]=2[CH3:15])[N:5]=[C:4]([NH:16][C:17]2[CH:35]=[CH:34][C:20]([CH2:21][O:22][C:23](=[O:33])[CH2:24][NH2:25])=[CH:19][CH:18]=2)[N:3]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 6344DichloromethaneHCID 8857Ethyl AcetateHCID 690158312-Tert-butoxycarbonylamino-acetic acid 4-[4-amino-6-(5-chloro-2-methyl-phenyl)-[1,3,5]triazin-2-yl-amino]-benzyl ester

생성물 1

HCID 10135531Amino-acetic acid 4-[4-amino-6-(5-chloro-2-methyl-phenyl)-[1,3,5]triazin-2ylamino]-benzyl ester수율 84%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A mixture of 2-tert-butoxycarbonylamino-acetic acid 4-[4-amino-6-(5-chloro-2-methyl-phenyl)-[1,3,5]triazin-2-yl-amino]-benzyl ester (1.0 g, 2 mmol), dichloromethane (20 ml), and a solution of hydrogen chloride in 1,4-dioxane (4 M, 5 ml) was stirred for 12 hours. The reaction mixture was poured into ethyl acetate (100 ml). The solid filtered and dried under reduced pressure to provide the hydrochloride salt of the title compound (0.38 g, 84% yield). 1H NMR (CD3OD) δ 7.75-8 (br s, 2H), 7.74 (s, 1H), 7.56-7.43 (m, 6H), 5.36 (s, 2H) 3.67 (s, 2H) 2.58 (s, 3H).

후처리

  1. filtrationThe solid filtered
  2. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-19da8372567049a9b8860173349e541e
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07618968B2

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