Ethyl Acetoacetate → HCID 178429550, 화합물

HRID 220000

반응식

HRID 220000 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([NH:9][NH:10][C:11](=[O:13])[CH3:12])[CH:5]=[CH:6][C:7]=1[Cl:8].[C:14](OCC)(=O)[CH2:15]C(C)=O.P(Cl)(Cl)Cl>>[Cl:1][C:2]1[CH:3]=[C:4]([N:9]2[C:14]([CH3:15])=[CH:12][C:11]([OH:13])=[N:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8]

참가 물질

4

반응물 3

HCID 8868Ethyl AcetoacetateHCID 24387Phosphorus trichlorideHCID 612829Acetic Acid N'-(3,4-Dichlorophenyl)hydrazide

생성물 1

HCID 178429550HCID 178429550, 화합물수율 41.3%

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온도
50 °C

실험 절차

To a mixture of (V) (5.0 g, 22.8 mmol) and ethyl acetoacetate (2.97 g 22.8 mmol) was slowly added PCl3 (3.13 g, 22.8 mmol). The mixture was warmed to 50° C. for 1.5 h, poured into ice water (150 ml), and the resulting precipitate was collected on a sintered glass funnel and recrystallized from EtOH to yield (VI) (2.29 g, 41%) as white crystals, mp 208-211° C. (lit. 208-209° C.), TLC CHCl3/MeOH 9:1.

후처리

  1. customthe resulting precipitate was collected on a sintered glass funnel
  2. customrecrystallized from EtOH

출처 및 근거

ORD 기록
ord-0c97f8adbe654658923d88615202f0ac
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08202872B2

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