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Hydrochloric Acid → Amino acetic acid-4-[2-amino-6-(5-chloro-2-ethoxy-phenyl)-pyrimidin-4-ylamino]-benzyl ester

HRID 28578
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인쇄 미리보기

반응식

HRID 28578 반응식
[NH2:1][C:2]1[N:7]=[C:6]([NH:8][C:9]2[CH:27]=[CH:26][C:12]([CH2:13][O:14][C:15](=[O:25])[CH2:16][NH:17]C(OC(C)(C)C)=O)=[CH:11][CH:10]=2)[CH:5]=[C:4]([C:28]2[CH:33]=[C:32]([Cl:34])[CH:31]=[CH:30][C:29]=2[O:35][CH2:36][CH3:37])[N:3]=1.Cl>C(OCC)(=O)C.O1CCOCC1>[NH2:1][C:2]1[N:7]=[C:6]([NH:8][C:9]2[CH:10]=[CH:11][C:12]([CH2:13][O:14][C:15](=[O:25])[CH2:16][NH2:17])=[CH:26][CH:27]=2)[CH:5]=[C:4]([C:28]2[CH:33]=[C:32]([Cl:34])[CH:31]=[CH:30][C:29]=2[O:35][CH2:36][CH3:37])[N:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 68983979Tert-butoxycarbonylamino-acetic acid 4-[2-amino-6-(5-chloro-2-ethoxy-phenyl)-pyrimidin-4-ylamino]-benzyl ester

생성물 1

HCID 11235689Amino acetic acid-4-[2-amino-6-(5-chloro-2-ethoxy-phenyl)-pyrimidin-4-ylamino]-benzyl ester수율 48%

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 31275
1,4-Dioxane
용매

실험 절차

A solution of tert-butoxycarbonylamino-acetic acid 4-[2-amino-6-(5-chloro-2-ethoxy-phenyl)-pyrimidin-4-ylamino]-benzyl ester in ethyl acetate (15 ml) was treated with a solution of hydrogen chloride in dioxane (4.0 M, 15 ml). After stirring for 16 hours, the solid was filtered and dried under reduced pressure to provide the hydrochloride salt of the title compound (0.273 g, 48% yield). 1H NMR (DMSO-d6) δ 1.39 (t, 3H, J=6.4 Hz, CH3), 3.89 (d, 2H, J=4.9 Hz, CH2), 4.17 (q, 2H, J=6.2 Hz, CH2), 5.25 (s, 2H, CH2), 6.70 (s, 1H, Ar), 7.28 (d, 1H, J=8.7 Hz, Ar), 7.46 (d, 2H, J=8.4 Hz, Ar), 7.62-7.67 (m, 2H, Ar), 7.88 (d, 2H, J=7.4 Hz, Ar), 8.37 (s, 3H), 11.10 (s, 1H), 12.68 (s, 1H).

후처리

  1. filtrationthe solid was filtered
  2. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-f99af370631c41c190313fe2b2841e29
출처 데이터셋
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07419984B2

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