Diisopropylamine → 2-(2-Hydroxy-2-p-methoxyphenylethyl)-6-methylpyrazine

HRID 443333

反応式

HRID 443333 の反応式
C(NC(C)C)(C)C.C([Li])CCC.[CH3:13][C:14]1[CH:19]=[N:18][CH:17]=[C:16]([CH3:20])[N:15]=1.[CH3:21][O:22][C:23]1[CH:30]=[CH:29][C:26]([CH:27]=[O:28])=[CH:25][CH:24]=1>CCOCC.CCCCCC.O>[OH:28][CH:27]([C:26]1[CH:29]=[CH:30][C:23]([O:22][CH3:21])=[CH:24][CH:25]=1)[CH2:13][C:14]1[CH:19]=[N:18][CH:17]=[C:16]([CH3:20])[N:15]=1

参加物

8

反応物 4

HCID 7912DiisopropylamineHCID 79382,6-DimethylpyrazineHCID 312444-MethoxybenzaldehydeHCID 178418339Butyllithium

生成物 1

HCID 5727552-(2-Hydroxy-2-p-methoxyphenylethyl)-6-methylpyrazine

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 3283Diethyl Ether溶媒3 回HCID 8058Hexane溶媒

実験手順

A solution of 5.05 grams (50 mmole) of diisopropylamine in 40 milliliters of ether was added to 47.1 mole butyllithium in hexane at 0° C. After stirring the resulting solution for 15 minutes, 5.4 grams (50 mmole) of 2,6-dimethylpyrazine in 50 milliliters of ether were added slowly and the reaction mixture was stirred at 0° C. for 30 minutes. A solution of 5.4 grams (40 mmole) of p-methoxybenzaldehyde in 40 milliliters of ether was added, and stirring at 0° C. was continued for an additional 30 minutes. Water was added, the organic phase was separated, washed with water and dried over magnesium sulfate.

後処理

  1. stirringthe reaction mixture was stirred at 0° C. for 30 minutes
  2. stirringstirring at 0° C.
  3. waitwas continued for an additional 30 minutes
  4. customthe organic phase was separated
  5. washwashed with water
  6. dry with materialdried over magnesium sulfate

出典と根拠

ORDレコード
ord-b78624bf854a48b6ac2689b539b97161
出典データセット
uspto-grants-1981_04
特許番号
US04259969

関連ノート

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