Water → HCID 18680340、化合物

HRID 2417287ノート

反応式

HRID 2417287 の反応式
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]

参加物

4

反応物 3

HCID 962WaterHCID 31215Triethyl phosphiteHCID 86585305HCID 86585305、化合物

生成物 1

HCID 18680340HCID 18680340、化合物収率 82%

実験手順

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): δ 7.06 (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).

後処理

  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.)

出典と根拠

ORDレコード
ord-2c4e791b13df42348044b0633b6d2f58
出典データセット
uspto-grants-2004_11
特許番号
US06825358B2

反応ノート

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