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HCID 18536675, 화합물 → HCID 18536678, 화합물

HRID 412046
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인쇄 미리보기

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HRID 412046 반응식
[CH2:1]([O:3][CH:4]([O:12][CH2:13][CH3:14])[C:5](=O)[CH:6]([CH3:10])[C:7](=O)[CH3:8])[CH3:2].C(=O)(O)[O-].[C:19]1([NH:25][C:26]([NH2:28])=[NH2+:27])[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1>C(O)C>[CH3:10][C:6]1[C:5]([CH:4]([O:12][CH2:13][CH3:14])[O:3][CH2:1][CH3:2])=[N:27][C:26]([NH:25][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[N:28][C:7]=1[CH3:8]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 18536675HCID 18536675, 화합물HCID 178512436HCID 178512436, 화합물

생성물 1

HCID 18536678HCID 18536678, 화합물수율 114.6%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
75 °C

실험 절차

A mixture of 44 g (purity about 50%, about 0.11 mol) of 1,1-diethoxy-3-methylpentane-2,4-dione (crude product, Example 2a) and 35 g (0.175 mol) of phenylguanidinium bicarbonate in 300 ml of ethanol was heated at 70-80° C. for about 3 hours. The reaction mixture was then concentrated and the residue was filtered, with suction, through silica gel using methyl tert-butyl ether. The solvent was evaporated. Less volatile components were distilled off under a pressure of 0.3 mbar, at a bath temperature of 150° C. The residue obtained was 38 g (quantitative yield) of the title compound as a yellow oil.

후처리

  1. concentrationThe reaction mixture was then concentrated
  2. filtrationthe residue was filtered, with suction, through silica gel
  3. customThe solvent was evaporated
  4. distillationLess volatile components were distilled off under a pressure of 0.3 mbar, at a bath temperature of 150° C
  5. customThe residue obtained

출처 및 근거

ORD 기록
ord-f34b6f5bfc144fff828b8d7d3e3917ff
출처 데이터셋
uspto-grants-2003_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06562833B1

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