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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Phosphoric Acid → HCID 12715053、化合物

HRID 2269587
ノート
印刷プレビュー

反応式

HRID 2269587 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[OH:9].[C:10]1([CH3:16])[CH:15]=[CH:14][CH:13]=CC=1.P(=O)(O)(O)O.C1CC=CC=1>C(C(C)=O)C(C)C.O1CCCC1>[CH3:1][C:2]1[CH:7]=[C:6]([CH:10]2[CH2:15][CH2:14][CH:13]=[CH:16]2)[CH:5]=[C:4]([CH3:8])[C:3]=1[OH:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 1004Phosphoric AcidHCID 1140Toluene2 回HCID 7612CyclopentadieneHCID 113352,6-Dimethylphenol

生成物 1

HCID 12715053HCID 12715053、化合物

試薬・触媒・溶媒 2

HCID 7909Methyl Isobutyl Ketone溶媒
HCID 8028
Tetrahydrofuran
溶媒

実験手順

Into a 2-liter flask having a stirrer, a condenser and a thermometer, 366 g of 2,6-dimethylphenol, 360 g of toluene and 102 g of phosphoric acid were introduced, and a solution of mixture of 247 g of cyclopentadiene and 200 g of toluene was added dropwise over a period of 3 hours while stirring the mixture under ice cooling, followed by further stirring for 4 hours at room temperature. To the reaction solution thus obtained, tetrahydrofuran (hereinafter “THF”) and methyl isobutyl ketone (hereinafter “MIBK”) were added, and the resultant solution was washed with water until it turned neutral, followed by distillation under reduced pressure. After the reaction solvent had evaporated, unreacted 2,6-dimethylphenol evaporated. A fraction at 3 mmHg and 140° C. was 2,6-dimethyl-4-(2-cyclopenten-1-yl)phenol. The results of analysis by GPC thereof are shown in FIG. 1. Its yield determined by GPC was 94% (area ratio).

後処理

  1. customInto a 2-liter flask having
  2. additionwas added dropwise over a period of 3 hours
  3. stirringby further stirring for 4 hours at room temperature
  4. customTo the reaction solution thus obtained
  5. washthe resultant solution was washed with water until it
  6. distillationfollowed by distillation under reduced pressure
  7. customAfter the reaction solvent had evaporated
  8. customunreacted 2,6-dimethylphenol evaporated
  9. customat 3 mmHg and 140° C.
  10. customThe results of analysis by GPC
  11. customIts yield

出典と根拠

ORDレコード
ord-3af76bcebf5548928505196d61a11dba
出典データセット
uspto-grants-2001_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06329492B1

反応ノート

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