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Ethylamine hydrochloride → N-(4-chloro-3-methylisothiazol-5-yl)-alpha-[(ethylamino)methylene]-[2-(2,2-dimeth-ylpropyl)benzoxazol-5-yl]acetamide

HRID 48153
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인쇄 미리보기

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HRID 48153 반응식
[Cl:1][C:2]1[C:3]([CH3:29])=[N:4][S:5][C:6]=1[NH:7][C:8](=[O:28])[C:9]([C:14]1[CH:15]=[CH:16][C:17]2[O:21][C:20]([CH2:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[N:19][C:18]=2[CH:27]=1)=[CH:10][N:11]([CH3:13])C.Cl.[CH2:31](N)C>O1CCCC1.O>[Cl:1][C:2]1[C:3]([CH3:29])=[N:4][S:5][C:6]=1[NH:7][C:8](=[O:28])[C:9]([C:14]1[CH:15]=[CH:16][C:17]2[O:21][C:20]([CH2:22][C:23]([CH3:25])([CH3:24])[CH3:26])=[N:19][C:18]=2[CH:27]=1)=[CH:10][NH:11][CH2:13][CH3:31]
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참가 물질

5

반응물 2

HCID 11198Ethylamine hydrochlorideHCID 69548266N-(4-chloro-3-methylisothiazol-5-yl)-alpha-[(dimethylamino)methylene]-[2-(2,2-dimethylpropyl)benzoxazol-5-yl]acetamide

생성물 1

HCID 69548595N-(4-chloro-3-methylisothiazol-5-yl)-alpha-[(ethylamino)methylene]-[2-(2,2-dimeth-ylpropyl)benzoxazol-5-yl]acetamide수율 85.4%

시약·촉매·용매 2

HCID 962Water용매
HCID 8028
Tetrahydrofuran
용매

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온도
60 °C

실험 절차

A mixture of N-(4-chloro-3-methylisothiazol-5-yl)-α-[(dimethylamino)methylene]-[2-(2,2-dimethylpropyl)benzoxazol-5-yl]acetamide (0.20 g, 0.00046 mole) [from Example 5] and ethylamine hydrochloride (0.0225 g, 0.0028 mole) in tetrahydrofuran (4 ml) and water (1 ml) was heated for 24 hours at 60° C. The mixture was cooled to room temperature, the solvent was evaporated in vacuo and the residue partitioned between ethyl acetate and saturated aqueous sodium bicarbonate solution. The organic extract was dried over anhydrous magnesium sulfate, filtered and the filtrate was evaporated in vacuo. Further purification by flash column chromatography, eluting with ethyl acetate:hexane at 2:3 by volume, gave N-(4-chloro-3-methylisothiazol-5-yl)-α-[(ethylamino)methylene]-[2-(2,2-dimeth-ylpropyl)benzoxazol-5-yl]acetamide as a colourless solid (0.17 g). Analysis by 1H NMR showed the product comprised a mixture of E- and Z-isomers.

후처리

  1. temperatureThe mixture was cooled to room temperature
  2. customthe solvent was evaporated in vacuo
  3. customthe residue partitioned between ethyl acetate and saturated aqueous sodium bicarbonate solution
  4. extractionThe organic extract
  5. dry with materialwas dried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. customthe filtrate was evaporated in vacuo
  8. customFurther purification by flash column chromatography
  9. washeluting with ethyl acetate

출처 및 근거

ORD 기록
ord-36922d85c99342c8a3007650d1e96f8c
출처 데이터셋
uspto-grants-2004_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06703347B2

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