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Tetrahydrofuran → HCID 23081948、化合物

HRID 1792082
ノート
印刷プレビュー

反応式

HRID 1792082 の反応式
[CH3:1][C:2]([CH3:5])([O-:4])[CH3:3].[K+].C([O:11][C:12]([N:14]1[CH2:19][CH2:18][N:17]([C:20]2[N:28]([C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][C:30]=3C=O)[C:27]3[C:26](=[O:37])[N:25]([CH2:38][O:39][C:40](=[O:45])[C:41]([CH3:44])([CH3:43])[CH3:42])[C:24](=[O:46])[N:23]([CH2:47][O:48][C:49](=[O:54])[C:50]([CH3:53])([CH3:52])[CH3:51])[C:22]=3[N:21]=2)[CH2:16][CH2:15]1)=O)(C)(C)C.O1CC[CH2:57][CH2:56]1>[Br-].C[P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.C(OCC)(=O)C>[C:2]([O:4][C:12]([N:14]1[CH2:19][CH2:18][N:17]([C:20]2[N:28]([C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][C:30]=3[CH:56]=[CH2:57])[C:27]3[C:26](=[O:37])[N:25]([CH2:38][O:39][C:40](=[O:45])[C:41]([CH3:43])([CH3:42])[CH3:44])[C:24](=[O:46])[N:23]([CH2:47][O:48][C:49](=[O:54])[C:50]([CH3:52])([CH3:53])[CH3:51])[C:22]=3[N:21]=2)[CH2:16][CH2:15]1)=[O:11])([CH3:5])([CH3:3])[CH3:1]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 8028Tetrahydrofuran2 回HCID 23536931HCID 23536931、化合物HCID 23665647Potassium tert-butoxide

生成物 1

HCID 23081948HCID 23081948、化合物

試薬・触媒・溶媒 2

HCID 74505Methyltriphenyliphosphonium bromide触媒HCID 8857
Ethyl Acetate
溶媒

実験手順

Methyltriphenylphosphonium bromide (3.52 g) was dissolved in tetrahydrofuran (20 ml), potassium tert-butoxide (948 mg) was added to the solution, and the mixture was stirred at room temperature for 1 hour. A solution of 4-[1,3-bis(2,2-dimethylpropionyloxymethyl)-7-(2-formylphenyl)-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-8-yl]piperazine-1-carboxylic acid tert-butyl ester (1.94 g) in tetrahydrofuran (20 ml) was added to the obtained reaction mixture at room temperature, and the mixture was stirred at room temperature for 3 hours and 50 minutes. The reaction mixture was diluted with ethyl acetate and washed with water. The organic layer was dried over anhydrous magnesium sulfate and filtered. The filtrate was concentrated under reduced pressure and the residue was purified by silica gel column chromatography to give 704 mg of the title compound from the elution fraction of hexane-ethyl acetate (2:1).

後処理

  1. stirringthe mixture was stirred at room temperature for 3 hours and 50 minutes
  2. washwashed with water
  3. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated under reduced pressure
  6. customthe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-43a4a930cbcd4fe4bd46bc76aade3211
出典データセット
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07074798B2

反応ノート

読み込み中…

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