Hydrochloric Acid → HCID 20378670、化合物

HRID 1390365ノート

反応式

HRID 1390365 の反応式
[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

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 516893Potassium BicarbonateHCID 203786594-Methyl-1-(2-nitrophenyl)piperazine-2-carboxylic acidHCID 178418361HCID 178418361、化合物

生成物 1

HCID 20378670HCID 20378670、化合物

試薬・触媒・溶媒 3

HCID 935Nickel触媒HCID 702Ethanol溶媒2 回HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-187c37c1d863497ab173ba520a58eaa9
出典データセット
uspto-grants-1979_02
特許番号
US04138567

反応ノート

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