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Hydrochloric Acid → HCID 178432906, 화합물

HRID 1580106
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HRID 1580106 반응식
[NH:1]1[CH:5]=[C:4]([S:6]([N:9]2[CH:13]=[CH:12][N:11]=[C:10]2[CH3:14])(=[O:8])=[O:7])[N:3]=[CH:2]1.[ClH:15]>C(O)C>[ClH:15].[NH:1]1[CH:5]=[C:4]([S:6]([N:9]2[CH:13]=[CH:12][N:11]=[C:10]2[CH3:14])(=[O:7])=[O:8])[N:3]=[CH:2]1
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 1784329051-(4-Imidazolylsulfonyl)-2-methylimidazole

생성물 1

HCID 178432906HCID 178432906, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 2.12 g of 1-(4-imidazolesulfonyl)-2-methylimidazole from Example 2 was dissolved in 100 ml of absolute ethanol in a dry flask equipped with a drying tube. A 50 ml aliquot of saturated ethereal hydrogen chloride was added over a five minute period. No precipitate formed immediately but did after about 15 minutes. The mixture was chilled in an ice bath for an additional 30 minutes and the precipitate filtered under a nitrogen atmosphere and dried under vacuum. The yield of white crystals of the hydrochloride of 1-(4-imidazolylsulfonyl)-2-methylimidazole was 1.87 g with mp 195°-8°. An analytical sample was made by recrystallization from ethanol and ether mixture, λmaxnujol 3.15-4.1 (NR3 +Cl-), 7.20 (SO2N) and 8.52 μ (SO2N).

후처리

  1. customequipped with a drying tube
  2. customNo precipitate formed immediately
  3. temperatureThe mixture was chilled in an ice bath for an additional 30 minutes
  4. filtrationthe precipitate filtered under a nitrogen atmosphere
  5. customdried under vacuum
  6. customAn analytical sample was made by recrystallization from ethanol and ether mixture, λmaxnujol 3.15-4.1 (NR3 +Cl-), 7.20 (SO2N) and 8.52 μ (SO2N)

출처 및 근거

ORD 기록
ord-13ab5a53d410486390f386bc21e6b1d0
출처 데이터셋
uspto-grants-1976_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03932444

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