1-{[N-(5,6-diphenylpyrazin-2-yl)-N-methylamino]methyl}-3-(methoxymethoxy)benzene → 3-{[N-(5,6-diphenylpyrazin-2-yl)-N-methylamino]methyl}phenol

HRID 1271283노트

반응식

HRID 1271283 반응식
[C:1]1([C:7]2[N:8]=[CH:9][C:10]([N:19]([CH2:21][C:22]3[CH:27]=[CH:26][CH:25]=[C:24]([O:28]COC)[CH:23]=3)[CH3:20])=[N:11][C:12]=2[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl.CO>CO>[C:1]1([C:7]2[N:8]=[CH:9][C:10]([N:19]([CH2:21][C:22]3[CH:23]=[C:24]([OH:28])[CH:25]=[CH:26][CH:27]=3)[CH3:20])=[N:11][C:12]=2[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

4

반응물 2

HCID 184526351-{[N-(5,6-diphenylpyrazin-2-yl)-N-methylamino]methyl}-3-(methoxymethoxy)benzeneHCID 21893726Hydrochloride methanol2회

생성물 1

HCID 184526533-{[N-(5,6-diphenylpyrazin-2-yl)-N-methylamino]methyl}phenol수율 81.2%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a suspension of 0.91 g of 1-{[N-(5,6-diphenylpyrazin-2-yl)-N-methylamino]methyl}-3-(methoxymethoxy)benzene in 10 ml of methanol, 2 ml of a 18% hydrogen chloride-methanol solution was added. After stirring at room temperature for 2 hours, 1 ml of a 18% hydrogen chloride-methanol solution was further added and the mixture was continuously stirred for one hour. After the solvent was evaporated under reduced pressure, the reaction solution was neutralized by adding an aqueous saturated sodium hydrogen carbonate solution and then extracted with ethyl acetate. The crude crystal was washed with diethyl ether and then dried to obtain 0.66 g of the desired compound as a colorless crystal having a melting point of 156 to 157° C.

후처리

  1. additionwas added
  2. stirringthe mixture was continuously stirred for one hour
  3. customAfter the solvent was evaporated under reduced pressure
  4. additionby adding an aqueous saturated sodium hydrogen carbonate solution
  5. extractionextracted with ethyl acetate
  6. washThe crude crystal was washed with diethyl ether
  7. customdried

출처 및 근거

ORD 기록
ord-eae735c6b94f4327aa4c2d6bfc8f2ce6
출처 데이터셋
uspto-grants-2007_04
특허 번호
US07205302B2

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