Hydrazine hydrate (1:1) → 6-[4-(3-Chloro-propoxy)-phenyl]-4,5-dihydro-2H-pyridazin-3-one

HRID 2042626노트

반응식

HRID 2042626 반응식
C([O:3][C:4](=O)[CH2:5][CH2:6][C:7]([C:9]1[CH:14]=[CH:13][C:12]([O:15][CH2:16][CH2:17][CH2:18][Cl:19])=[CH:11][CH:10]=1)=O)C.O.[NH2:22][NH2:23]>C(O)(C)C>[Cl:19][CH2:18][CH2:17][CH2:16][O:15][C:12]1[CH:13]=[CH:14][C:9]([C:7]2[CH2:6][CH2:5][C:4](=[O:3])[NH:22][N:23]=2)=[CH:10][CH:11]=1

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 596520284-[4-(3-Chloro-propoxy)-phenyl]-4-oxo-butyric acid ethyl ester

생성물 1

HCID 144418476-[4-(3-Chloro-propoxy)-phenyl]-4,5-dihydro-2H-pyridazin-3-one

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

In a 500 mL round bottom flask, 4-[4-(3-chloro-propoxy)-phenyl]-4-oxo-butyric acid ethyl ester (7.85 g, 26.3 mmol), and hydrazine monohydrate (2.55 mL, 52.7 mmol), in isopropanol (200 mL) was heated to reflux 14 h. The reaction was cooled and the solvent concentrated under vacuum. Purification with silica gel chromatography eluting with methylene chloride/methanol (95:5) produced 5.2 g (74%). MS m/z 267 (M+H).

후처리

  1. temperatureto reflux 14 h
  2. temperatureThe reaction was cooled
  3. concentrationthe solvent concentrated under vacuum
  4. customPurification with silica gel chromatography
  5. washeluting with methylene chloride/methanol (95:5)
  6. customproduced 5.2 g (74%)

출처 및 근거

ORD 기록
ord-4d21869709f84f5ca6b81d13ec2c28ea
출처 데이터셋
uspto-grants-2013_11
특허 번호
US08586588B2

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