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

HRID 399413

반응식

HRID 399413 반응식
[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]

참가 물질

8

반응물 4

HCID 313Hydrochloric Acid2회HCID 755984-Amino-3-methylbenzoic acidHCID 87820Ethyl 3-acetyl-4-oxopentanoateHCID 23668193Sodium Nitrite

생성물 1

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

시약·촉매·용매 3

HCID 702Ethanol용매2회HCID 962Water용매3회HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5b68ae39fb0d454b819718511809b210
출처 데이터셋
uspto-grants-1998_10
특허 번호
US05821243

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