Hydrochloric Acid → HCID 20378670, 화합물

HRID 2052108노트

반응식

HRID 2052108 반응식
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=2[N+:14]([O-])=O)[CH:4]([C:17]([OH:19])=O)[CH2:3]1.C(=O)(O)[O-].[K+].[H][H].Cl>[Ni].C(O)C.O>[CH3:1][N:2]1[CH2:7][CH2:6][N:5]2[C:8]3[C:9]([NH:14][C:17](=[O:19])[CH:4]2[CH2:3]1)=[CH:10][CH:11]=[CH:12][CH:13]=3

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 516893Potassium BicarbonateHCID 203786594-Methyl-1-(2-nitrophenyl)piperazine-2-carboxylic acidHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 20378670HCID 20378670, 화합물

시약·촉매·용매 3

HCID 935Nickel촉매HCID 702Ethanol용매2회HCID 962Water용매

실험 절차

A mixture of 3.5 g. (0.0135 mole) of 4-methyl-1-(o-nitrophenyl)piperazine-2-carboxylic acid, 2.5 g. (0.025 mole) of potassium bicarbonate, 110 ml. of water, 110 ml. of ethanol and 21/2 teaspoons of Raney nickel is hydrogenated in a Parr apparatus for 12 hours at an initial hydrogen pressure of 47 p.s.i. The catalyst is filtered and the filtrate is acidified with dilute hydrochloric acid. The mixture is then basified with sodium hydroxide and extracted with ethylacetate. The extract is dried and concentrated to give 2.3 g. of product. This is treated with 1 equivalent of hydrogen chloride in ethanol. After standing and cooling, filtration gives 2.4 g. of product, as the hydrochloride salt, m.p. 272°-275°. Recrystallization of the salt from ethanol-water gives 1.75 g., m.p. 284°-285° dec.

후처리

  1. additionA mixture of 3.5 g
  2. filtrationThe catalyst is filtered
  3. extractionextracted with ethylacetate
  4. customThe extract is dried
  5. concentrationconcentrated
  6. customto give 2.3 g
  7. temperaturecooling
  8. filtrationfiltration
  9. customgives 2.4 g
  10. customRecrystallization of the salt from ethanol-water
  11. customgives 1.75 g

출처 및 근거

ORD 기록
ord-98e2fd1395354b6686fd8ecb1803a35a
출처 데이터셋
uspto-grants-1980_01
특허 번호
US04182872

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