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Methanol → 2-(3-{5-[5-(1-Amino-1-methyl-ethyl)-pyridin-2-ylamino]-1-methyl-6-oxo-1,6-dihydro-pyridin-3-yl}-2-hydroxymethyl-phenyl)-6-tert butyl-8-fluoro-2H-phthalazin-1-one

HRID 2069866
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HRID 2069866 반응식
[NH2:1][C:2]([C:5]1[CH:6]=[CH:7][C:8]([NH:11][C:12]2[C:17](=[O:18])[N:16]([CH3:19])[CH:15]=[C:14]([C:20]3[CH:30]=[CH:29][CH:28]=[C:27]([N:31]4[N:40]=[CH:39][C:38]5[C:33](=[C:34]([F:45])[CH:35]=[C:36]([C:41]([CH3:44])([CH3:43])[CH3:42])[CH:37]=5)[C:32]4=[O:46])[C:21]=3[CH2:22][O:23]C(=O)C)[CH:13]=2)=[N:9][CH:10]=1)([CH3:4])[CH3:3].O.[OH-].[Li+].CO>O1CCOCC1>[NH2:1][C:2]([C:5]1[CH:6]=[CH:7][C:8]([NH:11][C:12]2[C:17](=[O:18])[N:16]([CH3:19])[CH:15]=[C:14]([C:20]3[C:21]([CH2:22][OH:23])=[C:27]([N:31]4[N:40]=[CH:39][C:38]5[C:33](=[C:34]([F:45])[CH:35]=[C:36]([C:41]([CH3:42])([CH3:43])[CH3:44])[CH:37]=5)[C:32]4=[O:46])[CH:28]=[CH:29][CH:30]=3)[CH:13]=2)=[N:9][CH:10]=1)([CH3:4])[CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 887MethanolHCID 168937Lithium hydroxide, monohydrateHCID 59473787Acetic acid 2-{5-[5-(1-amino-1-methyl-ethyl)-pyridin-2-ylamino]-1-methyl-6-oxo-1,6-dihydro-pyridin-3-yl}-6-(6-tert-butyl-8-fluoro-1-oxo-1H-phthalazin-2-yl)-benzyl ester

생성물 1

HCID 469089972-(3-{5-[5-(1-Amino-1-methyl-ethyl)-pyridin-2-ylamino]-1-methyl-6-oxo-1,6-dihydro-pyridin-3-yl}-2-hydroxymethyl-phenyl)-6-tert butyl-8-fluoro-2H-phthalazin-1-one수율 679.8%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

Acetic acid 2-{5-[5-(1-amino-1-methyl-ethyl)-pyridin-2-ylamino]-1-methyl-6-oxo-1,6-dihydro-pyridin-3-yl}-6-(6-tert-butyl-8-fluoro-1-oxo-1H-phthalazin-2-yl)-benzyl ester (159 mg, 0.0255 mmol) was dissolved in dioxane (3 ml). 2 M lithium hydroxide monohydrate solution (0.76 ml, 1.53 mmol) was added and stirred for 3hr at r.t. MeOH was added and the mixture purified purified by chromatography. Isolated product was dried under high vacuum at 50° C. to give 2-(3-{5-[5-(1-Amino-1-methyl-ethyl)-pyridin-2-ylamino]-1-methyl-6-oxo-1,6-dihydro-pyridin-3-yl}-2-hydroxymethyl-phenyl)-6-tert butyl-8-fluoro-2H-phthalazin-1-one (101 mg, 68%) as a off-white crystalline product. MS (H+)=583.3.

후처리

  1. customthe mixture purified
  2. custompurified by chromatography
  3. customIsolated product was dried under high vacuum at 50° C.

출처 및 근거

ORD 기록
ord-130e8ef3cfee4beba235b83ffb462320
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08299077B2

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