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Ammonia → HCID 3044138, 화합물

HRID 2419009
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HRID 2419009 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:14](O)[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.C1(C)C=CC(S(O)(=O)=O)=CC=1.O.N>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:3]=[C:4]([CH:14]=[CH: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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 222AmmoniaHCID 962Water2회HCID 6101p-Toluenesulfonic acidHCID 20316756HCID 20316756, 화합물

생성물 1

HCID 3044138HCID 3044138, 화합물수율 86.3%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

81 g of the compound produced in step (b) were dissolved in 500 ml of toluene and, to the solution so produced, was added a solution of 76 g of p-toluenesulphonic acid in the minimum quantity of water. The mixture was heated under reflux for about 20 hours, continuously removing the water formed. At the end of this time, the solution was cooled and poured into 2 liters of water, to which ammonia was added until the solution became alkaline. The organic phase was then separated, washed with water and dried with sodium sulphate. 66 g (yield 86%) of 3-chloro-4-cyclohexyl-1-(3-diethylamino-propen-1-yl)-benzene (hereinafter referred to as compound 933 CB) were obtained in the form of a light brown oil. This was dissolved in ether and reacted with a sufficient quantity of hydrochloric acid dissolved in the same solvent to produce 67 g of the hydrochloride having a melting point of 161° C.

후처리

  1. customso produced
  2. temperatureThe mixture was heated
  3. temperatureunder reflux for about 20 hours
  4. customcontinuously removing the water
  5. customformed
  6. temperatureAt the end of this time, the solution was cooled
  7. additionwas added until the solution
  8. customThe organic phase was then separated
  9. washwashed with water
  10. dry with materialdried with sodium sulphate

출처 및 근거

ORD 기록
ord-88d82667ea87424e91990b31e853998c
출처 데이터셋
uspto-grants-1978_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04104383

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