Ammonia → HCID 20433009, 화합물

HRID 371792노트

반응식

HRID 371792 반응식
[CH2:1]([O:7][C:8]1[CH:9]=[C:10]([CH:13]=[CH:14][C:15]=1[O:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH3:22])[CH:11]=O)[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].[NH3:23]>[Ni].C(O)C.[H][H]>[CH2:1]([O:7][C:8]1[CH:9]=[C:10]([CH:13]=[CH:14][C:15]=1[O:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH3:22])[CH2:11][NH2:23])[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6]

참가 물질

6

반응물 2

HCID 222AmmoniaHCID 118229373,4-dihexyloxybenzaldehyde

생성물 1

HCID 20433009HCID 20433009, 화합물수율 52.1%

시약·촉매·용매 3

HCID 935Nickel촉매HCID 702Ethanol용매HCID 178418361HCID 178418361, 화합물용매

실험 절차

Raney nickel (500 mg.), 3,4-dihexoxybenzaldehyde (6.12 g., 0.02 M) and ammonia (3.0 g., 0.177 M) in ethanol (100 ml.) are charged into a Paar shaker and hydrogenated at 40° C and an initial pressure of 51 psi. When approximately 20 psi drop in hydrogen pressure is observed, about 24 hours, the contents are removed and filtered. The filtrate is concentrated in vacuo to an amber oil which is dissolved in ethyl acetate (50 ml.). The solution is treated with ethyl acetate saturated with hydrogen chloride (100 ml.) and the resulting white hydrochloride salt collected; 3.7 g., m.p. 205°-206° C. The salt is then partitioned between chloroform (100 ml.) and saturated sodium bicarbonate solution (50 ml.). The chloroform phase is separated, washed with water (50 ml.), dried (Na2SO4) and concentrated to give 3,4-dihexoxybenzylamine as an oil; 3.2 g., 52.1% yield.

후처리

  1. customthe contents are removed
  2. filtrationfiltered
  3. concentrationThe filtrate is concentrated in vacuo to an amber oil which
  4. dissolutionis dissolved in ethyl acetate (50 ml.)
  5. additionThe solution is treated with ethyl acetate saturated with hydrogen chloride (100 ml.)
  6. customthe resulting white hydrochloride salt collected
  7. customThe salt is then partitioned between chloroform (100 ml.) and saturated sodium bicarbonate solution (50 ml.)
  8. customThe chloroform phase is separated
  9. washwashed with water (50 ml.)
  10. dry with materialdried (Na2SO4)
  11. concentrationconcentrated

출처 및 근거

ORD 기록
ord-af2ebda68d144d81bac7da12ed10244a
출처 데이터셋
uspto-grants-1978_05
특허 번호
US04087552

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