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Tetrahydrofuran → HCID 23081948, 화합물

HRID 1792082
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HRID 1792082 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 8028Tetrahydrofuran2회HCID 23536931HCID 23536931, 화합물HCID 23665647Potassium tert-butoxide

생성물 1

HCID 23081948HCID 23081948, 화합물

시약·촉매·용매 2

HCID 74505Methyltriphenyliphosphonium bromide촉매HCID 8857
Ethyl Acetate
용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-43a4a930cbcd4fe4bd46bc76aade3211
출처 데이터셋
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07074798B2

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