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Triethyl phosphite → HCID 15045704, 화합물

HRID 2372681
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HRID 2372681 반응식
[OH:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][C:3]=1[CH2:10]Cl.[P:12]([O:19]CC)([O:16][CH2:17][CH3:18])[O:13][CH2:14][CH3:15]>C(#N)C>[CH2:14]([O:13][P:12]([CH2:10][C:3]1[CH:4]=[C:5]([CH:6]=[O:7])[CH:8]=[CH:9][C:2]=1[OH:1])(=[O:19])[O:16][CH2:17][CH3:18])[CH3:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 31215Triethyl phosphite2회HCID 7140230Benzaldehyde, 3-(chloromethyl)-4-hydroxy-

생성물 1

HCID 15045704HCID 15045704, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

0.1 mole 4-Hydroxy-3-chloromethylbenzaldehyde was stirred in 75ml acetonitrile and 0.1 mole triethyl phosphite was added dropwise into the stirring suspension. After all the triethyl phosphite had been added, the reaction was refluxed for 4 hours. The reaction was then cooled to room temperature. The reaction solution was then filtered and the acetonitrile was removed on a rotary evaporator leaving behind a solid. This was recrystallized from THF:hexanes in a -20° C. freezer. The product was isolated on a buchner funnel and washed with -20° C. THF. mp 88°-88.5° C.

후처리

  1. temperaturethe reaction was refluxed for 4 hours
  2. filtrationThe reaction solution was then filtered
  3. customthe acetonitrile was removed on a rotary evaporator
  4. customleaving behind a solid
  5. customThis was recrystallized from THF
  6. customin a -20° C.
  7. customThe product was isolated on a buchner funnel
  8. washwashed with -20° C

출처 및 근거

ORD 기록
ord-8c80297d663b4dcf812dc066fb45752f
출처 데이터셋
uspto-grants-1992_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05100654

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