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Hydrochloric Acid → HCID 178432906、化合物

HRID 1580106
ノート
印刷プレビュー

反応式

HRID 1580106 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

HCID 178432906HCID 178432906、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-13ab5a53d410486390f386bc21e6b1d0
出典データセット
uspto-grants-1976_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03932444

反応ノート

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