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Ammonium Chloride → HCID 57701194, 화합물

HRID 602007
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HRID 602007 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:15]=[C:16]([O:22][CH3:23])[C:17]=1[O:18][CH2:19][C:20]#[CH:21])[C:6]([N:8]1[CH:14]2[CH:9]1[CH2:10][CH2:11][CH2:12][CH2:13]2)=[O:7].[Cl-:24].[NH4+]>[Cl-].[Zn+2].[Cl-].C(Cl)(Cl)Cl>[Cl:24][CH:14]1[CH2:13][CH2:12][CH2:11][CH2:10][CH:9]1[NH:8][C:6](=[O:7])[C:5]1[CH:4]=[C:3]([O:2][CH3:1])[C:17]([O:18][CH2:19][C:20]#[CH:21])=[C:16]([O:22][CH3:23])[CH:15]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 25517Ammonium ChlorideHCID 57701202HCID 57701202, 화합물

생성물 1

HCID 57701194HCID 57701194, 화합물

시약·촉매·용매 2

HCID 3007855Zincchloride촉매HCID 6212Chloroform용매2회

실험 절차

A mixture of 2 ml of chloroform and 258 mg of zinc (II) chloride was stirred at room temperature for 5 minutes. Thereafter, a mixture of 300 mg of 7-[3,5-dimethoxy-4-(2-propynyloxy)benzoyl]-7-azabicyclo[4.1.0]heptane and 2 ml of chloroform was added dropwise thereto at room temperature, and the resulting mixture was stirred at room temperature for 5 hours. Then, an aqueous saturated ammonium chloride solution was added to the reaction mixture, and this was extracted with chloroform. The organic layer was dried over magnesium sulfate, and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 0.16 g of N-(2-chlorocyclohexyl)-3,5-dimethoxy-4-(2-propynyloxy)benzamide (hereinafter, described as the compound 109 of the present invention) represented by the formula:

후처리

  1. additionwas added dropwise
  2. stirringat room temperature, and the resulting mixture was stirred at room temperature for 5 hours
  3. extractionthis was extracted with chloroform
  4. dry with materialThe organic layer was dried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-5700d92e6a9e48aab6382f4bd2487864
출처 데이터셋
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07902400B2

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