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Cyanamide → [4-Amino-2-[4-(2-dimethylaminoethoxy)-phenylamino]-thiazol-5-yl]-(3-methoxy-phenyl)-methanone

HRID 2415293
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HRID 2415293 반응식
[N:1]([C:4]1[CH:15]=[CH:14][C:7]([O:8][CH2:9][CH2:10][N:11]([CH3:13])[CH3:12])=[CH:6][CH:5]=1)=[C:2]=[S:3].[N:16]#[C:17][NH2:18].CC(C)([O-])C.[K+].Br[CH2:26][C:27]([C:29]1[CH:34]=[CH:33][CH:32]=[C:31]([O:35][CH3:36])[CH:30]=1)=[O:28]>C(#N)C.C(O)(C)(C)C.CCOCC.Cl.CCOCC>[NH2:16][C:17]1[N:18]=[C:2]([NH:1][C:4]2[CH:15]=[CH:14][C:7]([O:8][CH2:9][CH2:10][N:11]([CH3:12])[CH3:13])=[CH:6][CH:5]=2)[S:3][C:26]=1[C:27]([C:29]1[CH:34]=[CH:33][CH:32]=[C:31]([O:35][CH3:36])[CH:30]=1)=[O:28]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 4

HCID 9864CyanamideHCID 101294Bromomethyl 3-methoxyphenyl ketoneHCID 226409714-[2-(Dimethylamino)ethoxy]phenyl isothiocyanateHCID 23665647Potassium tert-butoxide

생성물 1

HCID 10001723[4-Amino-2-[4-(2-dimethylaminoethoxy)-phenylamino]-thiazol-5-yl]-(3-methoxy-phenyl)-methanone수율 42%

시약·촉매·용매 4

HCID 3283
Diethyl Ether
용매
HCID 6342Acetonitrile용매
HCID 6386tert-Butanol용매
HCID 10953452Ether hydrochloride용매

실험 절차

To a stirred mixture of [2-(4-isothiocyanato-phenoxy)-ethyl]-dimethylamine (0.6 g, 2.7 mmol) (from Step A) and cyanamide (0.123 g, 2.95 mmol) in acetonitrile (10 mL) and tert-butanol (10 mL), a solution of potassium tert-butoxide (2.7 mL, 1.0 M in tert-BuOH) was added. After 30 minutes at room temperature, 2-bromo-3′-methoxyacetophenone was added. The reaction mixture was stirred at room temperature for 1 hour and then refluxed for 1 hour. The chilled reaction mixture was diluted with ether and excess anhydrous hydrochloric acid/ether solution was added. The solids were filtered, washed with ether and then dissolved in dichloromethane/aqueous sodium bicarbonate. The dried (Na2SO4) organic solution was diluted with toluene (25 mL), concentrated, and refluxed to remove dichloromethane, The cooled mixture was diluted with hexane and filtered to give 0.47 g (42%) of [4-amino-2-[4-(2-dimethylaminoethoxy)-phenylamino]-thiazol-5-yl]-(3-methoxy-phenyl)-methanone as a yellow solid, mp 130° C. (dec). Mass spectrum (ES) MH+=413.

후처리

  1. temperaturerefluxed for 1 hour
  2. customThe chilled reaction mixture
  3. additionwas added
  4. filtrationThe solids were filtered
  5. washwashed with ether
  6. dissolutiondissolved in dichloromethane/aqueous sodium bicarbonate
  7. dry with materialThe dried (Na2SO4) organic solution
  8. additionwas diluted with toluene (25 mL)
  9. concentrationconcentrated
  10. temperaturerefluxed
  11. customto remove dichloromethane
  12. additionThe cooled mixture was diluted with hexane
  13. filtrationfiltered

출처 및 근거

ORD 기록
ord-aa9db080915744bb9a8fdb830efbbac9
출처 데이터셋
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06818663B2

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