Trimethyl phosphite → HCID 53693742, 화합물

HRID 2379027노트

반응식

HRID 2379027 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

HCID 53693742HCID 53693742, 화합물수율 97.8%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0fb972fbf37649cea934837c7452b477
출처 데이터셋
uspto-grants-1994_11
특허 번호
US05360797

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