N,N,N',N'-Tetramethylethylenediamine → HCID 19757216、化合物

HRID 1588160ノート

反応式

HRID 1588160 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH2:10][O:11][CH3:12])[C:6]([O:13][CH3:14])=[CH:5][C:4]=1[O:15][CH2:16][O:17][CH3:18].CN(C)CCN(C)C.[CH2:27]([Li])[CH2:28][CH2:29][CH3:30].ICCCC>C1(C)C=CC=CC=1.CN(C)P(=O)(N(C)C)N(C)C>[CH2:27]([C:8]1[C:7]([O:9][CH2:10][O:11][CH3:12])=[C:6]([O:13][CH3:14])[CH:5]=[C:4]([O:15][CH2:16][O:17][CH3:18])[C:3]=1[O:2][CH3:1])[CH2:28][CH2:29][CH3:30]

参加物

7

反応物 4

HCID 8037N,N,N',N'-TetramethylethylenediamineHCID 10962Butyl iodideHCID 10061046HCID 10061046、化合物HCID 178418339Butyllithium

生成物 1

HCID 19757216HCID 19757216、化合物

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 12679Hexamethylphosphoramide溶媒

実験手順

10 Grams of 1,4-dimethoxy-2,5-bis(methoxymethoxy)benzene was dissolved in 200 ml of anhydrous toluene under argon gas stream conditions, to this solution were added 50 ml of hexamethylphosphoric triamide and 8.75 ml of N,N,N',N'-tetramethylethylenediamine (TMEDA), and the mixture was cooled in a dry ice-acetone mixture bath. To this cooled mixture was added dropwise 39 ml of n-butyllithium (1.5 M, n-hexane solution), then stirred the mixture for 30 minutes. Next, 8.9 ml of 1-iodobutane was added to the reaction mixture, and the temperature was back to room temperature by taking for 12 hours. By procedures similar to those described in Reference Example 1, the above-mentioned reaction mixture was purified to obtain 8.5 g of 3-butyl-1,4-dimethoxy-2,5-bis(methoxymethoxy)benzene. Colorless oily substance.

後処理

  1. temperaturethe mixture was cooled in a dry ice-acetone mixture bath
  2. customwas back to room temperature
  3. waitby taking for 12 hours
  4. customthe above-mentioned reaction mixture was purified

出典と根拠

ORDレコード
ord-5b0304f00d6e410b979c27441099d89b
出典データセット
uspto-grants-1993_06
特許番号
US05220042

反応ノート

読み込み中…