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 1271283ノート

反応式

HRID 1271283 の反応式
[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

参加物

4

反応物 2

HCID 184526351-{[N-(5,6-diphenylpyrazin-2-yl)-N-methylamino]methyl}-3-(methoxymethoxy)benzeneHCID 21893726Hydrochloride methanol2 回

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-eae735c6b94f4327aa4c2d6bfc8f2ce6
出典データセット
uspto-grants-2007_04
特許番号
US07205302B2

反応ノート

読み込み中…