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Sodium Hydroxide → HCID 57456936, 화합물

HRID 2077024
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HRID 2077024 반응식
[C:1]([C:3]1[CH2:7][CH2:6][CH2:5][C:4]=1[NH:8][C:9]([NH:11]C(=O)C1C=CC=CC=1)=[O:10])#[N:2].[OH-].[Na+]>CCO>[NH2:2][C:1]1[C:3]2[CH2:7][CH2:6][CH2:5][C:4]=2[NH:8][C:9](=[O:10])[N:11]=1
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참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 57456937N-(2-cyanocyclopent-1-enylcarbamoyl)benzamide

생성물 1

HCID 57456936HCID 57456936, 화합물수율 68%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of N-(2-cyanocyclopent-1-enylcarbamoyl)benzamide (example 75a) (500 mg, 1.96 mmol) and NaOH (2 N, 2.7 mL) in EtOH (20 mL) was stirred at 100° C. under nitrogen for 2 hours. After cooling to room temperature, the clear reaction solution was filtered and the filtrate was carefully neutralized with 10% AcOH with vigorous stirring at 0° C. The resultant precipitate was collected by filtration, washed with warm water and then 20% EtOH in water to give the final product 4-amino-6,7-dihydro-1H-cyclopenta[d]pyrimidin-2(5H)-one (200 mg, 68%) as a white solid. 1H NMR (400 MHz, DMSO-d6) δ 10.57 (brs, 1H), 6.93 (brs, 1H), 6.65 (brs, 1H), 2.56 (t, J=7.2 Hz, 2H), 2.43 (t, J=7.6 Hz, 2H) 1.96-1.89 (m, 2H). MS 152 (MH+).

후처리

  1. filtrationthe clear reaction solution was filtered
  2. filtrationThe resultant precipitate was collected by filtration
  3. washwashed with warm water

출처 및 근거

ORD 기록
ord-6db6855841fb48808453cab0b7479b2f
출처 데이터셋
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07928111B2

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