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

HRID 451399

반응식

HRID 451399 반응식
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

참가 물질

4

반응물 2

HCID 2723790ThioureaHCID 127791292-Bromo-6-phenylcyclohexanone

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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)+].

후처리

  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

출처 및 근거

ORD 기록
ord-b582739d2f4d49828f147136e948ad00
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08486967B2

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