Dimethylformamide dimethyl acetal → HCID 86658932, 화합물

HRID 1950777노트

반응식

HRID 1950777 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([NH:11][C:12]2[C:17]([C:18]([O:20][CH2:21][CH3:22])=[O:19])=[C:16]([CH3:23])[N:15]=[C:14]([S:24][CH3:25])[N:13]=2)[CH:6]=[C:7]([O:9][CH3:10])[CH:8]=1.CO[CH:28](OC)[N:29]([CH3:31])[CH3:30]>CN(C=O)C.C(Cl)Cl.O>[CH3:10][O:9][C:7]1[CH:6]=[C:5]([NH:11][C:12]2[C:17]([C:18]([O:20][CH2:21][CH3:22])=[O:19])=[C:16](/[CH:23]=[CH:28]/[N:29]([CH3:31])[CH3:30])[N:15]=[C:14]([S:24][CH3:25])[N:13]=2)[CH:4]=[C:3]([O:2][CH3:1])[CH:8]=1

참가 물질

6

반응물 2

HCID 78373Dimethylformamide dimethyl acetalHCID 66984909HCID 66984909, 화합물

생성물 1

HCID 86658932HCID 86658932, 화합물수율 102%

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매

반응 조건

온도
130 °C

실험 절차

To the solution of ethyl 4-(3,5-dimethoxyphenylamino)-6-methyl-2(methylthio)pyrimidine-5-carboxylate (2.7 g, 7.4 mmol) in 30 mL DMF was added N,N-dimethylformamide dimethylacetal (1.58 mL, 11.1 mmol). The reaction mixture was stirred at 130° C. for 2 hour. After monitoring the reaction by TLC was cooled to room temperature, then the mixture was diluted with DCM and water. After extracted three times by DCM from the aqueous layer, the combined organic layer was dried over MgSO4. The solution was condensed under reduced pressure yielding crude mixture (3.16 g). The mixture was used for the next step without further purification.

후처리

  1. customthe reaction by TLC
  2. temperaturewas cooled to room temperature
  3. extractionAfter extracted three times by DCM from the aqueous layer
  4. dry with materialthe combined organic layer was dried over MgSO4
  5. customcondensed under reduced pressure

출처 및 근거

ORD 기록
ord-827148eb60c549d1b78e96cf0765cc2e
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08404677B2

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