Trimethyl phosphite → HCID 53693742、化合物

HRID 487888ノート

反応式

HRID 487888 の反応式
Br[CH2:2][C:3]1[C:12]([CH2:13]Br)=[CH:11][C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=1.C[O:16][P:17]([O:20][CH3:21])[O:18][CH3:19]>C1(C)C=CC=CC=1>[CH3:19][O:18][P:17]([CH2:2][C:3]1[C:12]([CH2:13][P:17](=[O:16])([O:20][CH3:21])[O:18][CH3:19])=[CH:11][C:10]2[C:5]([CH:4]=1)=[CH:6][CH:7]=[CH:8][CH:9]=2)(=[O:16])[O:20][CH3:21]

参加物

4

反応物 2

HCID 8472Trimethyl phosphiteHCID 2622592,3-Bis(bromomethyl)naphthalene

生成物 1

HCID 53693742HCID 53693742、化合物収率 97.8%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A flask is charged with 2,3-bis(bromomethyl)naphthalene (Example 22(b), 2.80 g, 8.9 mmol) and toluene (50 mL). The solution is heated at reflux and 25 mL of the toluene is collected in a Dean-Stark trap. The solution is then cooled to room temperature and trimethylphosphite (4.0 mL, 0.034 mol) is added. The reaction is heated to reflux temperature for 24 hours. The excess trimethylphosphite and toluene are removed at reduced pressure, giving a white solid (3.24 g). The solid is recrystallized from ethyl acetate-hexane to give 2.55 g of white crystals, mp 119.5°-120.5° C.

後処理

  1. temperatureThe solution is heated
  2. temperatureat reflux
  3. custom25 mL of the toluene is collected in a Dean-Stark trap
  4. temperatureThe reaction is heated
  5. temperatureto reflux temperature for 24 hours
  6. customThe excess trimethylphosphite and toluene are removed at reduced pressure

出典と根拠

ORDレコード
ord-b6ff4fede09d45659eea1b973a38a3ba
出典データセット
uspto-grants-1994_03
特許番号
US05298498

反応ノート

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