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Hydrochloric Acid → HCID 20478414、化合物

HRID 904675
ノート
印刷プレビュー

反応式

HRID 904675 の反応式
[Cl:1][C:2]1[C:11]2[CH:10]=[C:9]([O:12][CH3:13])[C:8]3[C:14](=[O:23])[CH:15]=[C:16]([C:18]([O:20]CC)=[O:19])[O:17][C:7]=3[C:6]=2[N:5]=[C:4]([C:24]([O:26]C)=[O:25])[CH:3]=1.Cl>C(O)(=O)C>[Cl:1][C:2]1[C:11]2[CH:10]=[C:9]([O:12][CH3:13])[C:8]3[C:14](=[O:23])[CH:15]=[C:16]([C:18]([OH:20])=[O:19])[O:17][C:7]=3[C:6]=2[N:5]=[C:4]([C:24]([OH:26])=[O:25])[CH:3]=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 20478384HCID 20478384、化合物

生成物 1

HCID 20478414HCID 20478414、化合物収率 34.5%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

To the product of step (e) (2.6 g) in glacial acetic acid (20 mls) was added concentrated hydrochloric acid (5.2 mls) and the whole was heated on a steam bath for three hours, during which time a solid slowly crystallised out of solution. The reaction mixture was cooled to room temperature and the crystallised solid was filtered off, washed thrice with glacial acetic acid and twice with diethyl ether. The resulting pale yellow solid was dried over sodium hydroxide pellets at 90° C. under a reduced pressure of 1 mm Hg for 2.5 hours, affording 0.8 g of the sub-title compound. N.M.R. Spectroscopy confirmed the structure.

後処理

  1. temperaturethe whole was heated on a steam bath for three hours, during which time a solid
  2. customslowly crystallised out of solution
  3. filtrationthe crystallised solid was filtered off
  4. washwashed thrice with glacial acetic acid
  5. dry with materialThe resulting pale yellow solid was dried over sodium hydroxide pellets at 90° C. under a reduced pressure of 1 mm Hg for 2.5 hours

出典と根拠

ORDレコード
ord-11d7c5c63b3f414ca17b7e268f0acee7
出典データセット
uspto-grants-1983_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04419352

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート