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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Phosphoric Acid → HCID 12715053, 화합물

HRID 2269587
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HRID 2269587 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 1004Phosphoric AcidHCID 1140Toluene2회HCID 7612CyclopentadieneHCID 113352,6-Dimethylphenol

생성물 1

HCID 12715053HCID 12715053, 화합물

시약·촉매·용매 2

HCID 7909Methyl Isobutyl Ketone용매
HCID 8028
Tetrahydrofuran
용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-3af76bcebf5548928505196d61a11dba
출처 데이터셋
uspto-grants-2001_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06329492B1

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