Acetic Anhydride → HCID 23552950, 화합물

HRID 2270971노트

반응식

HRID 2270971 반응식
[Cl-].[Al+3].[Cl-].[Cl-].[C:5](OC(=O)C)(=[O:7])[CH3:6].[Cl:12][CH2:13][C:14]([O:16][C:17]1[CH:25]=[C:24]2[C:20]([CH:21]=[CH:22][N:23]2[C:26](=[O:31])[C:27]([CH3:30])([CH3:29])[CH3:28])=[CH:19][CH:18]=1)=[O:15]>ClC(Cl)C>[C:5]([C:21]1[C:20]2[C:24](=[CH:25][C:17]([O:16][C:14](=[O:15])[CH2:13][Cl:12])=[CH:18][CH:19]=2)[N:23]([C:26](=[O:31])[C:27]([CH3:28])([CH3:30])[CH3:29])[CH:22]=1)(=[O:7])[CH3:6]

참가 물질

5

반응물 3

HCID 7918Acetic AnhydrideHCID 6451240Aluminum(III) ChlorideHCID 103796646-chloroacetoxy-1-pivaloylindole

생성물 1

HCID 23552950HCID 23552950, 화합물수율 36%

시약·촉매·용매 1

HCID 63651,1-Dichloroethane용매2회

실험 절차

To a suspension of 9.5 g (72 mmol) of aluminum chloride in dichloroethane (47.5 ml) was added dropwise 3.64 g (36 mmol) of acetic anhydride. After stirring for 15 min at room temperature, to the above mixture was added dropwise 3.3 g (11 mmol) of 6-chloroacetoxy-1-pivaloylindole (prepared in accordance with the literature (SYNTHESIS, p1018, 1994) in dichloroethane (33 ml). After stirring for 1 hour at room temperature, the mixture was poured into ice-water. The mixture was extracted with ethyl acetate. The extract was washed twice with water and aqueous sodium bicarbonate, and dried. The solution was concentrated and the obtained residue was chromatographed on silica gel (ethyl acetate as eluant) to give 1.23 g of 3-acetyl-6-chloroacetoxy-1-pivaloylindole as an oil. Yield: 36%.

후처리

  1. stirringAfter stirring for 1 hour at room temperature
  2. extractionThe mixture was extracted with ethyl acetate
  3. washThe extract was washed twice with water and aqueous sodium bicarbonate
  4. customdried
  5. concentrationThe solution was concentrated
  6. customthe obtained residue was chromatographed on silica gel (ethyl acetate as eluant)

출처 및 근거

ORD 기록
ord-764eef94fac04de694931c6140c15e5e
출처 데이터셋
uspto-grants-2001_12
특허 번호
US06333323B1

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