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Triethyl phosphite → HCID 15045704、化合物

HRID 2372681
ノート
印刷プレビュー

反応式

HRID 2372681 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 31215Triethyl phosphite2 回HCID 7140230Benzaldehyde, 3-(chloromethyl)-4-hydroxy-

生成物 1

HCID 15045704HCID 15045704、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8c80297d663b4dcf812dc066fb45752f
出典データセット
uspto-grants-1992_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05100654

反応ノート

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