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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
ノート
印刷プレビュー

反応式

HRID 2069866 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 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

生成物 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-one収率 679.8%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-130e8ef3cfee4beba235b83ffb462320
出典データセット
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08299077B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート