Butanoic acid, 2-(ethoxymethylene)-3-oxo-, ethyl ester → HCID 12194769, 화합물

HRID 917384

반응식

HRID 917384 반응식
Cl.[C:2]1([CH2:8][C:9]([NH2:11])=[NH:10])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:12]([C:15](=[CH:21]OCC)[C:16]([O:18][CH2:19][CH3:20])=[O:17])(=O)[CH3:13].C([O-])(=O)C.[Na+]>CN(C)C=O>[CH2:8]([C:9]1[N:11]=[C:12]([CH3:13])[C:15]([C:16]([O:18][CH2:19][CH3:20])=[O:17])=[CH:21][N:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 97734Butanoic acid, 2-(ethoxymethylene)-3-oxo-, ethyl esterHCID 517045Sodium AcetateHCID 124155142-Phenylethanimidamide hydrochloride

생성물 1

HCID 12194769HCID 12194769, 화합물수율 89%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
100 °C

실험 절차

To 100 ml of N,N-dimethylformamide, 17.1 g (100 mmol) of 2-phenylacetoamidine hydrochloric acid salt, synthesized in accordance with a method described in “Tetrahedron”, page 887 (1984), 18.6 g (100 mmol) of ethyl 2-acetyl-3-ethoxyacrylate and 9.0 g (110 mmol) of sodium acetate were suspended, followed by stirring at 100° C. for 3 hours. The reaction liquid was cooled and then poured into ice water, and extracting with diethyl ether. The organic layer was washed with water and a saturated saline solution in this order, followed by drying over anhydrous magnesium sulfate and concentrating under reduced pressure to obtain 22.8 g (yield: 89%) of ethyl 2-benzyl-4-methylpyrimidine-5-carboxylate.

후처리

  1. customThe reaction liquid
  2. temperaturewas cooled
  3. extractionextracting with diethyl ether
  4. washThe organic layer was washed with water
  5. dry with materialby drying over anhydrous magnesium sulfate
  6. concentrationconcentrating under reduced pressure

출처 및 근거

ORD 기록
ord-22aa77e03b3042448a53c53288fa8fe5
출처 데이터셋
uspto-grants-2007_09
특허 번호
US07273878B2

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