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Ammonia → HCID 23047741, 화합물

HRID 2107147
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HRID 2107147 반응식
[NH3:1].Cl[C:3]([CH:5]([CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][C:16]1[CH:21]=[CH:20][C:19]([Cl:22])=[CH:18][CH:17]=1)[C:6]([O:8][CH2:9][CH3:10])=[O:7])=[O:4]>C(Cl)Cl>[NH2:1][C:3]([CH:5]([CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][C:16]1[CH:21]=[CH:20][C:19]([Cl:22])=[CH:18][CH:17]=1)[C:6]([O:8][CH2:9][CH3:10])=[O:7])=[O:4]
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참가 물질

4

반응물 2

HCID 222AmmoniaHCID 23047721HCID 23047721, 화합물

생성물 1

HCID 23047741HCID 23047741, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A saturated solution of gaseous ammonia in 25 ml of methylene chloride is added drop by drop at -10° C. to a solution of 5.6 (17 mmol) of ethyl 2-(chlorocarbonyl)-7-(4-chlorophenyl)heptanoate in 50 ml of methylene chloride. The mixture is stirred for 30 minutes at room temperature, suction filtered from the ammonium chloride, the filtrate is washed with water, and dried and concentrated. The concentrate is chromatographed on silica gel with a mixture of toluene and dioxane (5:1). 3.6 g (68% of theory) is obtained of ethyl 2-(aminocarbonyl)-7-(4-chlorophenyl)heptanoate, M.P. 110°-111° C.

후처리

  1. filtrationsuction filtered from the ammonium chloride
  2. washthe filtrate is washed with water
  3. customdried
  4. concentrationconcentrated
  5. customThe concentrate is chromatographed on silica gel with a mixture of toluene and dioxane (5:1)

출처 및 근거

ORD 기록
ord-f8378a0353fb4b69b3024e2568fc3b7f
출처 데이터셋
uspto-grants-1990_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04933367

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