Acetic Acid → HCID 68217647, 화합물

HRID 1661055노트

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HRID 1661055 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[O:11][CH3:12])[C:7](=O)[CH2:6][CH2:5]2.[C:14]([CH2:16][C:17]([O:19][CH2:20][CH3:21])=[O:18])#[N:15].CC(O)=O.C([O-])(=O)C.[NH4+]>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[O:11][CH3:12])/[C:7](=[C:16](\[C:14]#[N:15])/[C:17]([O:19][CH2:20][CH3:21])=[O:18])/[CH2:6][CH2:5]2

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 7764Ethyl cyanoacetateHCID 517165Ammonium AcetateHCID 109214765-Chloro-6-methoxy-1-indanone

생성물 1

HCID 68217647HCID 68217647, 화합물수율 62%

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
120 °C

실험 절차

To the solution of 5-chloro-6-methoxy-2,3-dihydro-1H-inden-1-one (Prep15, 12 g, 61.2 mmol) in toluene (240 ml) was added ethyl cyanoacetate (8.3 g, 73.46 mmol), AcOH (48 ml, 0.8 mol) and ammonium acetate (12 g, 0.16 mol). The mixture was stirred for 12 hours at 120° C., checked by TLC, concentrated, filtered and washed with water and ethanol twice and purified by FC to afford 11 g of title compound (y=62%).

후처리

  1. concentrationconcentrated
  2. filtrationfiltered
  3. washwashed with water and ethanol twice
  4. custompurified by FC

출처 및 근거

ORD 기록
ord-6d5a1f520e3e4784be214b4193ac042d
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08030322B2

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