1,4-Dioxane hydrochloride → 4-{2-[2-(Acetylamino)-1,3-thiazol-4-yl]ethyl}phenyl hydrazinecarboxylate hydrochloride

HRID 1892471노트

반응식

HRID 1892471 반응식
[NH:1]([C:10]([O:12][C:13]1[CH:18]=[CH:17][C:16]([CH2:19][CH2:20][C:21]2[N:22]=[C:23]([NH:26][C:27](=[O:29])[CH3:28])[S:24][CH:25]=2)=[CH:15][CH:14]=1)=[O:11])[NH:2]C(OC(C)(C)C)=O.O1CCOCC1.[ClH:36]>ClCCl>[ClH:36].[NH:1]([C:10]([O:12][C:13]1[CH:14]=[CH:15][C:16]([CH2:19][CH2:20][C:21]2[N:22]=[C:23]([NH:26][C:27](=[O:29])[CH3:28])[S:24][CH:25]=2)=[CH:17][CH:18]=1)=[O:11])[NH2:2]

참가 물질

4

반응물 2

HCID 204431481,4-Dioxane hydrochlorideHCID 866499784-{2-[2-(Acetylamino)-1,3-thiazol-4-yl]ethyl}phenyl tert-butyl hydrazine-1,2-dicarboxylate

생성물 1

HCID 866499794-{2-[2-(Acetylamino)-1,3-thiazol-4-yl]ethyl}phenyl hydrazinecarboxylate hydrochloride수율 100.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a suspension of 4-{2-[2-(acetylamino)-1,3-thiazol-4-yl]ethyl}phenyl tert-butyl hydrazine-1,2-dicarboxylate (445.2 mg, 1.06 mmol) in anhydrous dichloromethane (5.3 ml) was added 4M hydrogen chloride dioxane solution (5.3 ml, 21.3 mmol). After stirring at room temperature for 2 hr, the reaction mixture was concentrated under reduced pressure. Ethyl acetate was added to the concentrated residue, and the mixture was concentrated again under reduced pressure. This operation was performed 3 times to remove hydrogen chloride gas azeotropically. The residue was suspended in ethyl acetate, and the solid was collected by filtration, washed twice with ethyl acetate, and dried under reduced pressure to give the title compound (380.5 mg, quantitative) as a white solid.

후처리

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. additionEthyl acetate was added to the concentrated residue
  3. concentrationthe mixture was concentrated again under reduced pressure
  4. customto remove hydrogen chloride gas azeotropically
  5. filtrationthe solid was collected by filtration
  6. washwashed twice with ethyl acetate
  7. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-7bf8475ec6bf4b959787fd7323278f6e
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08507690B2

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