Hydrochloric Acid → Ethyl 3-(4-carboxy-2-methylphenylhydrazono)-4-oxopentanoate

HRID 399413

反応式

HRID 399413 の反応式
[NH2:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][C:3]=1[CH3:11].Cl.[N:13]([O-])=O.[Na+].[C:17]([CH:20](C(=O)C)[CH2:21][C:22]([O:24][CH2:25][CH3:26])=[O:23])(=[O:19])[CH3:18]>O.C(O)C.N1C=CC=CC=1>[CH3:11][C:3]1[CH:4]=[C:5]([CH:9]=[CH:10][C:2]=1[NH:1][N:13]=[C:20]([C:17](=[O:19])[CH3:18])[CH2:21][C:22]([O:24][CH2:25][CH3:26])=[O:23])[C:6]([OH:8])=[O:7]

参加物

8

反応物 4

HCID 313Hydrochloric Acid2 回HCID 755984-Amino-3-methylbenzoic acidHCID 87820Ethyl 3-acetyl-4-oxopentanoateHCID 23668193Sodium Nitrite

生成物 1

HCID 86751496Ethyl 3-(4-carboxy-2-methylphenylhydrazono)-4-oxopentanoate

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒2 回HCID 962Water溶媒3 回HCID 1049Pyridine溶媒

実験手順

A mixture of 3 g. (19.8 mmol) of 4-amino-3-methylbenzoic acid in 50 ml. of water and 50 ml. of ethanol and 3.56 ml. of concentrated hydrochloric acid was cooled in an ice bath and then 1.5 g. of NaNO2 (21.8 mmol.) in 10 ml. of water was added portionwise. The mixture was allowed to come to room temperature and then added to a solution of 4.06 g. (21.8 mmol.) of ethyl 3-acetyl-4-oxopentanoate and 8 ml. of pyridine in 25 ml. of ethanol. The reaction mixture was left for 24 hours at room temperature with stirring. The mixture was acidified with concentrated hydrochloric acid and diluted with 20 ml. of water. The resulting solid was collected and washed with water and pentane to yield 5.2 g.

後処理

  1. additionA mixture of 3 g
  2. customto come to room temperature
  3. additionadded to a solution of 4.06 g
  4. additiondiluted with 20 ml
  5. customThe resulting solid was collected
  6. washwashed with water and pentane
  7. customto yield 5.2 g

出典と根拠

ORDレコード
ord-5b68ae39fb0d454b819718511809b210
出典データセット
uspto-grants-1998_10
特許番号
US05821243

関連ノート

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