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Hydrochloric Acid → (+/-)-1,4-Bis(diphenylcarbamoyl)piperazine2-carboxylic acid

HRID 486751
ノート
印刷プレビュー

反応式

HRID 486751 の反応式
[C:1]1([N:7]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[C:8](Cl)=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl.Cl.[NH:19]1[CH2:24][CH2:23][NH:22][CH2:21][CH:20]1[C:25]([OH:27])=[O:26].[OH-:28].[Na+].Cl>C(#N)C>[C:1]1([N:7]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[C:8]([N:19]2[CH2:24][CH2:23][N:22]([C:8](=[O:28])[N:7]([C:1]3[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=3)[C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)[CH2:21][CH:20]2[C:25]([OH:27])=[O:26])=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 65741N,N-Diphenylcarbamic chlorideHCID 2723757Piperazine-2-carboxylic acid dihydrochloride

生成物 1

HCID 22004705(+/-)-1,4-Bis(diphenylcarbamoyl)piperazine2-carboxylic acid収率 26%

試薬・触媒・溶媒 1

HCID 6342
Acetonitrile
溶媒

実験手順

A solution of 946 mg (4 mmole) of 98% diphenylcarbamoyl chloride in 4 ml of acetonitrile was added dropwise to a stirring solution of 406.2 mg (2 mmole) of piperazine-2-carboxylic acid dihydrochloride [E. Felder, S. Maffei, S. Pietra and D. Pitre, Helv. Chim., Acta. 43, 888 (1960)] in 4 ml of 2.5N-sodium hydroxide at a temperature between 0° and 5° C. After the addition was completed, the stirring was continued for 4 hours and the solution was acidified with 2N-hydrochloric acid while cooling in an ice bath. The reaction mixture was concentrated under reduced pressure and the residue was extracted with chloroform. After washing with water, the chloroform solution was dried over MgSO4 and concentrated in vacuo. The only product which solidified on cooling was triturated with isopropyl ether to give 270 mg (26%) of (±)-1,4-bis(diphenylcarbamoyl)piperazine2-carboxylic acid, m.p. 244°-246° C.

後処理

  1. additionAfter the addition
  2. temperaturewhile cooling in an ice bath
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. extractionthe residue was extracted with chloroform
  5. washAfter washing with water
  6. dry with materialthe chloroform solution was dried over MgSO4
  7. concentrationconcentrated in vacuo
  8. temperatureon cooling
  9. customwas triturated with isopropyl ether

出典と根拠

ORDレコード
ord-e4ed22f95ff544038c73676c772e5fa1
出典データセット
uspto-grants-1994_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05292726

反応ノート

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