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

HRID 2419772
ノート
印刷プレビュー

反応式

HRID 2419772 の反応式
[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]
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 962WaterHCID 1004Phosphoric AcidHCID 6557IsopreneHCID 79333-Chlorophenol

生成物 1

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

試薬・触媒・溶媒 2

HCID 7108Phenothiazine触媒
HCID 7239
1,2-Dichlorobenzene
溶媒

実験手順

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##

後処理

  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

出典と根拠

ORDレコード
ord-049ecd6e8eff416991056ebddebe3169
出典データセット
uspto-grants-1978_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04107324

反応ノート

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