3,4,5-Trimethoxybenzonitrile → HCID 178487380、化合物

HRID 870531

反応式

HRID 870531 の反応式
[CH3:1][C:2]1[N:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=O.C(O)C.C(=O)=O.C([N-]C(C)C)(C)C.[Li+].[CH3:25][O:26][C:27]1[CH:28]=[C:29]([CH:32]=[C:33]([O:37][CH3:38])[C:34]=1[O:35][CH3:36])[C:30]#[N:31]>O1CCCC1.O>[CH3:38][O:37][C:33]1[CH:32]=[C:29]([C:30]2[N:31]=[C:4]([OH:6])[C:3]3[CH:7]=[CH:8][CH:9]=[N:10][C:2]=3[CH:1]=2)[CH:28]=[C:27]([O:26][CH3:25])[C:34]=1[O:35][CH3:36]

参加物

7

反応物 4

HCID 158923,4,5-TrimethoxybenzonitrileHCID 6433732-Methylnicotinic acidHCID 2724682Lithium diisopropylamideHCID 19604758Methanedione--ethanol (1/1)

生成物 1

HCID 178487380HCID 178487380、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
0 °C

実験手順

7 g 2-Methyl-nicotinic acid was suspended in 150 mL of tetrahydrofuran, and cooled to −70° C. with a bath of ethanol/dry ice. 80 mL lithium diisopropylamide (2.0 M in tetrahydrofuran/n-heptane/ethylbenzene) was added dropwise over 10 min and the mixture was stirred for 2 h at 0° C. Then it was cooled to −73° C. and a solution of 10 g 3,4,5-trimethoxy-benzonitrile (4.24) in 50 mL tetrahydrofuran was added. Then the reaction mixture was warmed overnight to ambient temperature. 30 mL Water was added and the solvent was distilled off before 200 mL ethyl acetate was added and the precipitate that formed was collected.

後処理

  1. temperatureThen it was cooled to −73° C.
  2. temperatureThen the reaction mixture was warmed overnight to ambient temperature
  3. distillationthe solvent was distilled off before 200 mL ethyl acetate
  4. additionwas added
  5. customthe precipitate that formed
  6. customwas collected

出典と根拠

ORDレコード
ord-78e6103bd710448bb48c3fe0d82c9112
出典データセット
uspto-grants-2015_03
特許番号
US08969568B2

関連ノート

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