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Water → 7-Chloro-3,3-dimethyl-2,3-dihydro-1H-inden-5-ol

HRID 2419772
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HRID 2419772 반응식
[CH2:1]=[CH:2][C:3](=[CH2:5])[CH3:4].[Cl:6][C:7]1[CH:8]=[C:9]([OH:13])[CH:10]=[CH:11][CH:12]=1.P(=O)(O)(O)O.O>ClC1C=CC=CC=1Cl.C1C2NC3C(=CC=CC=3)SC=2C=CC=1>[Cl:6][C:7]1[CH:8]=[C:9]([OH:13])[CH:10]=[C:11]2[C:12]=1[CH2:1][CH2:2][C:3]2([CH3:5])[CH3:4]
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참가 물질

7

반응물 4

HCID 962WaterHCID 1004Phosphoric AcidHCID 6557IsopreneHCID 79333-Chlorophenol

생성물 1

HCID 30175517-Chloro-3,3-dimethyl-2,3-dihydro-1H-inden-5-ol수율 16.4%

시약·촉매·용매 2

HCID 7108Phenothiazine촉매
HCID 7239
1,2-Dichlorobenzene
용매

실험 절차

449 g of isoprene, stabilized with 1.35 g of phenothiazine, were added dropwise over the course of 5.5 hours to a solution of 771 g of m-chlorophenol, 77 g of 85% strength phosphoric acid and 6 ml of water in 1.44 liters of o-dichlorobenzene at 150° C. To complete the reaction, stirring was continued overnight at 150° C. After cooling, the acid phase was separated off and extracted by shaking with toluene. The combined organic phases were washed until neutral. Fractional distillation gives 194 g of 7-chloro-3,3-dimethyl-5-hydroxy-indane; boiling point 105°-110° C/0.5 mm Hg; melting point 86.5° - 87.5° C. ##STR38##

후처리

  1. customthe reaction
  2. temperatureAfter cooling
  3. customthe acid phase was separated off
  4. extractionextracted
  5. stirringby shaking with toluene
  6. washThe combined organic phases were washed until neutral
  7. distillationFractional distillation

출처 및 근거

ORD 기록
ord-049ecd6e8eff416991056ebddebe3169
출처 데이터셋
uspto-grants-1978_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04107324

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