Water → (E)-N-ethyl-N-(2-penten-4-ynyl)-2-[2-[3-(3-thienyl)phenoxy]ethoxy]ethylamine

HRID 1756174

반응식

HRID 1756174 반응식
[CH2:1]([N:3]([CH2:13][CH2:14][O:15][CH2:16][CH2:17][O:18][C:19]1[CH:24]=[CH:23][CH:22]=[C:21]([C:25]2[CH:29]=[CH:28][S:27][CH:26]=2)[CH:20]=1)[CH2:4]/[CH:5]=[CH:6]/[C:7]#[C:8][Si](C)(C)C)[CH3:2].C(OCC)(=O)C.O>CO.O1CCCC1.[F-].[K+]>[CH2:1]([N:3]([CH2:13][CH2:14][O:15][CH2:16][CH2:17][O:18][C:19]1[CH:24]=[CH:23][CH:22]=[C:21]([C:25]2[CH:29]=[CH:28][S:27][CH:26]=2)[CH:20]=1)[CH2:4]/[CH:5]=[CH:6]/[C:7]#[CH:8])[CH3:2]

참가 물질

7

반응물 3

HCID 962WaterHCID 8857Ethyl AcetateHCID 19917013(E)-N-ethyl-N-(5-trimethylsilyl-2-penten-4-ynyl)-2-[2-[3-(3-thienyl)phenoxy]ethoxy]ethylamine

생성물 1

HCID 19917041(E)-N-ethyl-N-(2-penten-4-ynyl)-2-[2-[3-(3-thienyl)phenoxy]ethoxy]ethylamine수율 78.2%

시약·촉매·용매 3

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매HCID 522689Potassium Fluoride용매

실험 절차

2.0 g of the resulting allylamine compound was dissolved in a mixture of methanol (5 ml) and tetrahydrofuran (5 ml), and 10 ml of a saturated aqueous solution of potassium fluoride was added. The mixture was stirred overnight at room temperature, and then ethyl acetate and water were added. The organic layer separated was worked up in a customary manner, and the product was purified by silica gel column chromatography [methylene chloride/methanol=100/1] to give 1.3 g of (E)-N-ethyl-N-(2-penten-4-ynyl)-2-[2-[3-(3-thienyl)phenoxy]ethoxy]ethylamine as a colorless oil.

후처리

  1. additionwas added
  2. customThe organic layer separated
  3. customthe product was purified by silica gel column chromatography [methylene chloride/methanol=100/1]

출처 및 근거

ORD 기록
ord-d22b8a90a9b6490289afc8a4116b7dcf
출처 데이터셋
uspto-grants-1995_08
특허 번호
US05439932

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