N,N,N',N'-Tetramethylethylenediamine → HCID 19757216, 화합물

HRID 1588160노트

반응식

HRID 1588160 반응식
[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]

참가 물질

7

반응물 4

HCID 8037N,N,N',N'-TetramethylethylenediamineHCID 10962Butyl iodideHCID 10061046HCID 10061046, 화합물HCID 178418339Butyllithium

생성물 1

HCID 19757216HCID 19757216, 화합물

시약·촉매·용매 2

HCID 1140Toluene용매HCID 12679Hexamethylphosphoramide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5b0304f00d6e410b979c27441099d89b
출처 데이터셋
uspto-grants-1993_06
특허 번호
US05220042

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