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3-Chloro-4-cyclohexyl-1-(3-diethylamino-1-oxo-propyl)-benzene → HCID 20316756, 화합물

HRID 2419008
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HRID 2419008 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:14](=[O:22])[CH2:15][CH2:16][N:17]([CH2:20][CH3:21])[CH2:18][CH3:19])[CH:5]=[CH:6][C:7]=1[CH:8]1[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1.[B-].[Na+]>CO.C(=O)([O-])[O-].[Na+].[Na+]>[Cl:1][C:2]1[CH:3]=[C:4]([CH:14]([OH:22])[CH2:15][CH2:16][N:17]([CH2:20][CH3:21])[CH2:18][CH3:19])[CH:5]=[CH:6][C:7]=1[CH:8]1[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1
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참가 물질

5

반응물 2

HCID 203167583-Chloro-4-cyclohexyl-1-(3-diethylamino-1-oxo-propyl)-benzeneHCID 22959485Vertellus2회

생성물 1

HCID 20316756HCID 20316756, 화합물수율 77%

시약·촉매·용매 2

HCID 887Methanol용매HCID 10340Sodium Carbonate용매

실험 절차

116 g of the product of step (a) were suspended in a mixture of 1 liter of methanol and 60 ml of 40% sodium carbonate. 40 g of sodium borohydrate were then added slowly to this suspension, maintaining the temperature below 8° C. After all of the sodium borohydrate had been added, the mixture was left for 12 hours at ambient temperature, after which 1.5 liters of 5% soda solution were added and the mixture was extracted with 700 ml of isopropyl ether. The organic phase was washed with water, dried over sodium sulphate and then evaporated to dryness. 81 g (yield 77% of theory) of 3-chloro-4-cyclohexyl-1-(3-diethylamino-1-hydroxy-propyl)-benzene were obtained in the form of a yellow oil.

후처리

  1. temperaturemaintaining the temperature below 8° C
  2. additionafter which 1.5 liters of 5% soda solution were added
  3. extractionthe mixture was extracted with 700 ml of isopropyl ether
  4. washThe organic phase was washed with water
  5. dry with materialdried over sodium sulphate
  6. customevaporated to dryness

출처 및 근거

ORD 기록
ord-e1a77c6c671f4a5d87375d72d34f3534
출처 데이터셋
uspto-grants-1978_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04104383

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