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Hydrochloric Acid → 4-[7-(2-Butynyl)-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-8-yl]piperazine-1-carboxylic acid tert-butyl ester

HRID 1792061
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인쇄 미리보기

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HRID 1792061 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[N:22]([CH2:23][C:24]#[C:25][CH3:26])[C:21]3[C:20](=[O:27])[N:19](COC(=O)C(C)(C)C)[C:18](=[O:36])[N:17](COC(=O)C(C)(C)C)[C:16]=3[N:15]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[H-].[Na+].Cl>O1CCCC1.CO>[C:1]([O:5][C:6]([N:8]1[CH2:9][CH2:10][N:11]([C:14]2[N:22]([CH2:23][C:24]#[C:25][CH3:26])[C:21]3[C:20](=[O:27])[NH:19][C:18](=[O:36])[NH:17][C:16]=3[N:15]=2)[CH2:12][CH2:13]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
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참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 24758Sodium hydrideHCID 235369404-[7-(2-Butynyl)-1,3-bis-(2,2-dimethylpropionyloxymethyl)-2,6-dioxo 2,3,6,7-tetrahydro-1H-purin-8-yl]piperazine-1-carboxylic acid tert-butyl ester

생성물 1

HCID 235369444-[7-(2-Butynyl)-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-8-yl]piperazine-1-carboxylic acid tert-butyl ester수율 100.3%

시약·촉매·용매 2

HCID 887
Methanol
용매
HCID 8028Tetrahydrofuran용매

실험 절차

4-[7-(2-Butynyl)-1,3-bis-(2,2-dimethylpropionyloxymethyl)-2,6-dioxo 2,3,6,7-tetrahydro-1H-purin-8-yl]piperazine-1-carboxylic acid tert-butyl ester (1.9 g) was dissolved in a solvent mixture of tetrahydrofuran (20 ml) and methanol (10 ml), and sodium hydride (0.31 g) was added to the solution. The mixture was stirred at room temperature for 1 hour. The reaction mixture was neutralized with 2 N hydrochloric acid and extracted with ethyl acetate. The organic layer was concentrated by distillation to give 1.2 g of the title compound.

후처리

  1. additionwas added to the solution
  2. extractionextracted with ethyl acetate
  3. concentrationThe organic layer was concentrated by distillation

출처 및 근거

ORD 기록
ord-4c2fdca0ce324394835b646a0e3e9743
출처 데이터셋
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07074798B2

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