Lithium hydride → HCID 15700630, 화합물

HRID 236780

반응식

HRID 236780 반응식
[CH:1]([NH:3][C:4]1[C:5]2[CH:18]=[CH:17][CH:16]=[CH:15][C:6]=2[S:7][C:8]=1[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)=O.[H-].[Li+].[Al].[Li].[H-].[Al+3].[H-].[H-]>O1CCOCC1.C(Cl)Cl.O>[CH3:1][NH:3][C:4]1[C:5]2[CH:18]=[CH:17][CH:16]=[CH:15][C:6]=2[S:7][C:8]=1[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1

참가 물질

9

반응물 5

HCID 62714Lithium hydrideHCID 3028194LithiumHCID 5359268AluminumHCID 15700625HCID 15700625, 화합물HCID 21584524Aluminiumhydride

생성물 1

HCID 15700630HCID 15700630, 화합물

시약·촉매·용매 3

HCID 962Water용매HCID 6344Dichloromethane용매HCID 312751,4-Dioxane용매

실험 절차

3.0 g (11.8 mmol) of 3-formamido-2-phenyl-benzo(b)thiophene and 1.08 g (28.4 mmol) of lithium hydride and aluminium are refluxed with stirring for 30 minutes in 60 milliliters of absolute dioxane. The cooled reaction mixture is mixed with water to decompose the excess lithium and aluminium hydride and, after the addition of approximately 100 milliliters of CH2Cl2, it is stirred for a further 15 minutes. After centrifuging with the addition of the hyflo, the organic phase is dried over K2CO3 and evaporated: 3-methylamino-2-phenyl-benzo(b)thiophene in the form of a crude oily product. It is dissolved in a little CHCl3 and converted into the hydrochloride by hydrochloric gas: 2.6 g (80% of theory) of colourless crystals in a mixture of ethanol and ether, decomposition from 198° C. (in sealed tubes).

후처리

  1. customThe cooled reaction mixture
  2. additionAfter centrifuging with the addition of the hyflo
  3. dry with materialthe organic phase is dried over K2CO3
  4. customevaporated
  5. dissolutionIt is dissolved in a little CHCl3
  6. addition2.6 g (80% of theory) of colourless crystals in a mixture of ethanol and ether, decomposition from 198° C. (in sealed tubes)

출처 및 근거

ORD 기록
ord-646c84d9ff4b4925bdf2e6ad448a3cd5
출처 데이터셋
uspto-grants-1979_06
특허 번호
US04157399

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