Thiourea → 4-Phenyl-4,5,6,7-tetrahydrobenzo[d]thiazol-2-amine

HRID 451399

反応式

HRID 451399 の反応式
Br[CH:2]1[CH2:7][CH2:6][CH2:5][CH:4]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[C:3]1=O.[NH2:15][C:16]([NH2:18])=[S:17]>CCO>[C:8]1([CH:4]2[C:3]3[N:15]=[C:16]([NH2:18])[S:17][C:2]=3[CH2:7][CH2:6][CH2:5]2)[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

参加物

4

反応物 2

HCID 2723790ThioureaHCID 127791292-Bromo-6-phenylcyclohexanone

生成物 1

HCID 866566974-Phenyl-4,5,6,7-tetrahydrobenzo[d]thiazol-2-amine収率 93.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 2-bromo-6-phenyl-cyclohexanone (4.32 g, 17 mmol) and thiourea (1.18 g, 16 mmol) in EtOH (150 mL) was heated to reflux for 12 hours. The solvent was evaporated, diethyl ether was added to the residue and stirred at room temperature for 1 hour, the solid filtered off and washed with diethylether. The solid was dissolved in ethyl acetate and the organic phase was washed three times with sodium carbonate solution. The organic phase was dried over sodium sulfate, the solvent was evaporated to give the title compound as a white solid (3.46 g, 88%). MS ISP (m/e): 231.1 [(M+H)+].

後処理

  1. temperatureto reflux for 12 hours
  2. customThe solvent was evaporated
  3. additiondiethyl ether was added to the residue
  4. filtrationthe solid filtered off
  5. washwashed with diethylether
  6. dissolutionThe solid was dissolved in ethyl acetate
  7. washthe organic phase was washed three times with sodium carbonate solution
  8. dry with materialThe organic phase was dried over sodium sulfate
  9. customthe solvent was evaporated

出典と根拠

ORDレコード
ord-b582739d2f4d49828f147136e948ad00
出典データセット
uspto-grants-2013_07
特許番号
US08486967B2

関連ノート

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