Water → HCID 18680340, 화합물

HRID 2227854노트

반응식

HRID 2227854 반응식
Br[CH2:2][CH2:3][CH2:4][CH2:5][C-:6]1[CH2:10][CH:9]=[CH:8][S:7]1.O.[CH2:12]([O:14][P:15]([O:19]CC)[O:16][CH2:17][CH3:18])[CH3:13]>>[CH2:12]([O:14][P:15]([CH2:2][CH2:3][CH2:4][CH2:5][C:6]1[S:7][CH:8]=[CH:9][CH:10]=1)(=[O:19])[O:16][CH2:17][CH3:18])[CH3:13]

참가 물질

4

반응물 3

HCID 962WaterHCID 31215Triethyl phosphiteHCID 86585305HCID 86585305, 화합물

생성물 1

HCID 18680340HCID 18680340, 화합물수율 82%

실험 절차

A solution of 1d (4.58 g, 0.02 mol) in 20 mL of triethylphosphite was heated at 160° C. for 20 hours, with nitrogen bubbling directly into the solution. The solution was cooled to room temperature and 50 mL of water was added; the resulting mixture was stirred for 4 hours. The product was extracted with methylene chloride, the organic layer was separated and washed with brine, then dried over anhydrous magnesium sulfate. Evaporation of the solvent yielded an oily residue, which was distilled under vacuum (0.12 mm Hg, 135° C.) to give 1e as a colorless oil (6.0 g, 82%). 1H NMR (250 MHz, 25° C., CDCl3): δ7.06 (m, 1H, Ar—H), 6.85 (m, 1H, Ar—H), 6.72 (m, 1H, Ar—H), 4.03 (m, 4H, POCH2CH3), 2.79 (t, 2H, Ar—CH2), 1.72 (m, 6H, CH2CH2CH2P), 1.26 (t, 6H, POCH2CH3).

후처리

  1. extractionThe product was extracted with methylene chloride
  2. customthe organic layer was separated
  3. washwashed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customEvaporation of the solvent
  6. customyielded an oily residue, which
  7. distillationwas distilled under vacuum (0.12 mm Hg, 135° C.)

출처 및 근거

ORD 기록
ord-56e471ccad6447bd8d77db862f11d8a5
출처 데이터셋
uspto-grants-2002_07
특허 번호
US06414164B1

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