2-Bromo-1-[3,5-di(tert-butyl)-4-hydroxyphenyl]ethan-1-one → Phenol, 2,6-bis(1,1-dimethylethyl)-4-(2H-imidazo(2,1-b)(1,3,4)thiadiazin-3-yl)-, hydrochloride

HRID 329385

反応式

HRID 329385 の反応式
Br[CH2:2][C:3]([C:5]1[CH:10]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[C:8]([OH:15])=[C:7]([C:16]([CH3:19])([CH3:18])[CH3:17])[CH:6]=1)=O.[ClH:20].[NH2:21][N:22]1[CH:26]=[CH:25][N:24]=[C:23]1[SH:27]>C(O)C>[ClH:20].[C:16]([C:7]1[CH:6]=[C:5]([C:3]2[CH2:2][S:27][C:23]3=[N:24][CH:25]=[CH:26][N:22]3[N:21]=2)[CH:10]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[C:8]=1[OH:15])([CH3:19])([CH3:18])[CH3:17]

参加物

4

反応物 2

HCID 6161612-Bromo-1-[3,5-di(tert-butyl)-4-hydroxyphenyl]ethan-1-oneHCID 178479588HCID 178479588、化合物

生成物 1

HCID 3088381Phenol, 2,6-bis(1,1-dimethylethyl)-4-(2H-imidazo(2,1-b)(1,3,4)thiadiazin-3-yl)-, hydrochloride

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 18.0 g (0.055 mol) of 2-bromo-1-(3,5-ditert.butyl-4-hydroxyphenyl)-ethanone and 7.6 g (0.05 mol) of 1-amino-2-mercaptoimidazole hydrochloride from step (a) in 150 ml of ethanol was refluxed for 9 hours. The residue remaining after evaporation of the solution was rendered alkaline by means of 50 ml of 2N sodium hydroxide solution and extracted with chloroform. In order to convert the product into the hydrochloride, an equimolar amount of ethereal hydrochloric acid was added to the dried chloroform phase, and the batch of crystals produced was filtered off under suction and crystallized from ethanol.

後処理

  1. customafter evaporation of the solution
  2. extractionextracted with chloroform
  3. additionan equimolar amount of ethereal hydrochloric acid was added to the dried chloroform phase
  4. customthe batch of crystals produced
  5. filtrationwas filtered off under suction
  6. customcrystallized from ethanol

出典と根拠

ORDレコード
ord-23ca300e63234258a42542ff377dfc38
出典データセット
uspto-grants-1990_01
特許番号
US04891374

関連ノート

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