Hydrazine hydrate (1:1) → HCID 178526464, 화합물

HRID 490312노트

반응식

HRID 490312 반응식
C[O:2][C:3](=O)[C:4]1[CH:9]=[CH:8][C:7]([N+:10]([O-:12])=[O:11])=[CH:6][C:5]=1F.O.[NH2:16][NH2:17]>C(O)C>[N+:10]([C:7]1[CH:6]=[C:5]2[C:4]([C:3]([OH:2])=[N:16][NH:17]2)=[CH:9][CH:8]=1)([O-:12])=[O:11]

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)2회HCID 3013872Methyl 2-fluoro-4-nitrobenzoate

생성물 1

HCID 178526464HCID 178526464, 화합물수율 30.9%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

2-Fluoro-4-nitrobenzoic acid methyl ester (5 g, 25.11 mmol) and hydrazine hydrate (1.34 ml, 27.62 mmol) were dissolved in 250 ml of ethanol and heated under reflux for 11 h. A further 0.26 ml of hydrazine hydrate were added and heated under reflux for a further 6 h, and the mixture was concentrated and ethyl acetate and water were added. The precipitated residue was filtered off with suction and dried. Purification by preparative HPLC (PR18, acetonitrile/water 0.1% TFA) resulted in 1.39 g of product, M+H+: 180.05.

후처리

  1. temperatureheated
  2. temperatureunder reflux for 11 h
  3. temperatureheated
  4. temperatureunder reflux for a further 6 h
  5. concentrationthe mixture was concentrated
  6. additionethyl acetate and water were added
  7. filtrationThe precipitated residue was filtered off with suction
  8. customdried
  9. customPurification by preparative HPLC (PR18, acetonitrile/water 0.1% TFA)

출처 및 근거

ORD 기록
ord-3dba0618625249d08a951b4b74fccaa1
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07528155B2

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