HCID 18368343, 화합물 → HCID 9884882, 화합물

HRID 379696노트

반응식

HRID 379696 반응식
C(OC([NH:8][CH2:9][CH2:10][O:11][C:12]1[CH:30]=[CH:29][C:15]([NH:16][C:17](=[O:28])[C:18]2[C:23]([O:24][CH3:25])=[CH:22][CH:21]=[CH:20][C:19]=2[O:26][CH3:27])=[CH:14][CH:13]=1)=O)(C)(C)C.Cl.O1CCOCC1>>[NH2:8][CH2:9][CH2:10][O:11][C:12]1[CH:30]=[CH:29][C:15]([NH:16][C:17](=[O:28])[C:18]2[C:19]([O:26][CH3:27])=[CH:20][CH:21]=[CH:22][C:23]=2[O:24][CH3:25])=[CH:14][CH:13]=1

참가 물질

3

반응물 2

HCID 18368343HCID 18368343, 화합물HCID 204431481,4-Dioxane hydrochloride

생성물 1

HCID 9884882HCID 9884882, 화합물수율 83.3%

실험 절차

4′-[2-(tert-Butoxycarbonylamino)ethoxy]-2,6-dimethoxybenzanilide (1.17 g) was added with 4N HCl/dioxane (5 ml) and mixed for 6 hours at room temperature. The reaction mixture was concentrated under vacuum and residue was dissolved into chloroform (50 ml). The solution was washed with 1N sodium hydroxide aqueous solution (10 ml) followed by saturated sodium chloride (20 ml). After concentration under vacuum to small volume, the solution was subjected to purification by silica-gel column chromatography (chloroform methanol=4:1) to obtain 4′-(2-aminoethoxy)-2,6-dimethoxybenzanilide (0.74 g) as white powder.

후처리

  1. additionmixed for 6 hours at room temperature
  2. concentrationThe reaction mixture was concentrated under vacuum and residue
  3. dissolutionwas dissolved into chloroform (50 ml)
  4. washThe solution was washed with 1N sodium hydroxide aqueous solution (10 ml)
  5. concentrationAfter concentration under vacuum to small volume
  6. customthe solution was subjected to purification by silica-gel column chromatography (chloroform methanol=4:1)

출처 및 근거

ORD 기록
ord-99ba9c1f3c4f480ea9a3c9bb1a06c07d
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06300368B1

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