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tert-Butanol → HCID 136173745、化合物

HRID 2079223
ノート
印刷プレビュー

反応式

HRID 2079223 の反応式
[CH3:1][N:2]([CH3:45])[C:3]([CH2:5][O:6][C:7]1[C:8]([F:44])=[C:9]([CH:15]([NH:31][C:32]2[CH:37]=[CH:36][C:35]([C:38]3[N:42]=[C:41]([CH3:43])[O:40][N:39]=3)=[CH:34][CH:33]=2)[C:16]2[NH:20][C:19](=[O:21])[N:18]([C:22]3[CH:30]=[CH:29][CH:28]=[CH:27][C:23]=3C(O)=O)[N:17]=2)[CH:10]=[C:11]([CH2:13][CH3:14])[CH:12]=1)=[O:4].C([N:48]([CH2:51]C)CC)C.C1(P(N=[N+]=[N-])(C2C=CC=CC=2)=[O:60])C=CC=CC=1.C(OCC)(=O)C.[C:76]([OH:80])([CH3:79])([CH3:78])[CH3:77]>O>[C:76]([O:80][C:51](=[O:60])[NH:48][C:23]1[CH:27]=[CH:28][CH:29]=[CH:30][C:22]=1[N:18]1[C:19](=[O:21])[NH:20][C:16]([CH:15]([C:9]2[CH:10]=[C:11]([CH2:13][CH3:14])[CH:12]=[C:7]([O:6][CH2:5][C:3](=[O:4])[N:2]([CH3:45])[CH3:1])[C:8]=2[F:44])[NH:31][C:32]2[CH:37]=[CH:36][C:35]([C:38]3[N:42]=[C:41]([CH3:43])[O:40][N:39]=3)=[CH:34][CH:33]=2)=[N:17]1)([CH3:79])([CH3:78])[CH3:77]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 6386tert-ButanolHCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 199401P,P-Diphenylphosphinic azideHCID 136173790HCID 136173790、化合物

生成物 1

HCID 136173745HCID 136173745、化合物

試薬・触媒・溶媒 1

HCID 962
Water
溶媒

実験手順

A solution of 0.320 g of 2-(3-{(3-dimethylcarbamoylmethoxy-5-ethyl-2-fluorophenyl)-[4-(5-methyl-[1,2,4]oxadiazol-3-yl)phenylamino]methyl}-5-oxo-4,5-dihydro-1H-[1,2,4]triazol-1-yl)benzoic acid, 0.098 ml of triethylamine and 0.151 ml of diphenylphosphorylazide in 10 ml of t-butanol was stirred under a nitrogen atmosphere at room temperature for 20 hours and then at 70° C. for 36 hours. After adding 100 ml of ethyl acetate and 50 ml of water to the reaction mixture, the organic layer was dried over anhydrous magnesium sulfate, the desiccating agent was filtered off and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (methanol-ethyl acetate) to give the title compound (0.135 g) as a white solid.

後処理

  1. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  2. filtrationthe desiccating agent was filtered off
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (methanol-ethyl acetate)

出典と根拠

ORDレコード
ord-423c169db232453999ff73cc322c3302
出典データセット
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07928228B2

反応ノート

読み込み中…

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