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Sodium Bicarbonate → HCID 15616694, 화합물

HRID 330301
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HRID 330301 반응식
[Br:1][C:2]1[N:6]2[C:7]([CH3:15])=[C:8]([CH2:13][CH3:14])[C:9]([O:11][CH3:12])=[N:10][C:5]2=[N:4][C:3]=1[C:16](=[O:27])[C:17]#[C:18][CH2:19][O:20]C1CCCCO1.C(=O)(O)[O-].[Na+]>CO.Cl>[Br:1][C:2]1[N:6]2[C:7]([CH3:15])=[C:8]([CH2:13][CH3:14])[C:9]([O:11][CH3:12])=[N:10][C:5]2=[N:4][C:3]=1[C:16](=[O:27])[C:17]#[C:18][CH2:19][OH:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 516892Sodium BicarbonateHCID 19989901HCID 19989901, 화합물

생성물 1

HCID 15616694HCID 15616694, 화합물수율 32.1%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 887Methanol용매

실험 절차

A solution of 5.0 g (11.5 mmol) of 1-(3-bromo-6-ethyl-7-methoxy-5-methylimidazo[1,2-a]pyrimidin-2-yl)-4-(tetrahydropyran-2-yloxy)-2-butyn-1-one in a mixture of 100 ml of methanol and 35 ml of 2N hydrochloric acid stood at room temperature for 30 minutes and then was neutralized with aqueous sodium bicarbonate. Extraction with chloroform gave an oil which was chromatographed over silica (chloroform: ether: methanol 100:0:0 gradually changing to 0:95:5) to obtain 1.3 g (32%) of 1-(3-bromo-6-ethyl-7-methoxy-5-methylimidazo[1,2-a]pyrimidin-2-yl)-4-hydroxy-2-butyn-1-one as off-white crystals melting at 212°-3° C. (decomp.).

후처리

  1. extractionExtraction with chloroform
  2. customgave an oil which
  3. customwas chromatographed over silica (chloroform: ether: methanol 100:0:0

출처 및 근거

ORD 기록
ord-bc18ae89b8244dd0a19c4dd2254351b5
출처 데이터셋
uspto-grants-1990_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04895866

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