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

반응식

HRID 329385 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-23ca300e63234258a42542ff377dfc38
출처 데이터셋
uspto-grants-1990_01
특허 번호
US04891374

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