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Hydrogen Bromide → HCID 21561613, 화합물

HRID 1581133
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인쇄 미리보기

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HRID 1581133 반응식
COC([O:5][C:6]1[C:7]([CH3:18])=[N:8][CH:9]=[C:10]([CH2:12][O:13][C:14]([O:16][CH3:17])=[O:15])[CH:11]=1)=O.Br.C(=O)(O)[O-].[Na+]>C(O)C>[CH3:17][O:16][C:14]([O:13][CH2:12][C:10]1[CH:11]=[C:6]([OH:5])[C:7]([CH3:18])=[N:8][CH:9]=1)=[O:15]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 260Hydrogen BromideHCID 516892Sodium BicarbonateHCID 21561588HCID 21561588, 화합물

생성물 1

HCID 21561613HCID 21561613, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
90 °C

실험 절차

A solution of 1 g. of 3-methoxycarbonyloxy-5-methoxycarbonyloxymethyl-2-methylpyridine in an aqueous ethanol (10 ml. of ethanol and 5 ml. of water) was adjusted to pH 1-1.5 with 10% hydrobromic acid. The mixture was heated at 90°C for 30 minutes, then cooled and neutralized with sodium bicarbonate and extracted with ethyl acetate. The extract was dried over anhydrous sodium sulfate and concentrated into a small volume and the addition of n-hexane gave 0.45 g. of the desired product as colorless crystals melting at 187°-189°C, which showed no depression of melting point on admixture with the authentic sample and the IR spectrum coincided with that of the standard completely.

후처리

  1. temperaturecooled
  2. extractionextracted with ethyl acetate
  3. dry with materialThe extract was dried over anhydrous sodium sulfate
  4. concentrationconcentrated into a small volume
  5. additionthe addition of n-hexane
  6. customgave 0.45 g

출처 및 근거

ORD 기록
ord-dd239861ed674cd599bc466206cc2840
출처 데이터셋
uspto-grants-1976_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03935311

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