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Guaiacol → 6-Methoxy-3,3-dimethylindan-5-ol

HRID 2419769
ノート
印刷プレビュー

反応式

HRID 2419769 の反応式
[CH2:1]=[CH:2][C:3](=[CH2:5])[CH3:4].[C:6]1([O:13][CH3:14])[C:7](=[CH:9][CH:10]=[CH:11][CH:12]=1)[OH:8].P(=O)(O)(O)O.O>C1(C)C(C)=CC=CC=1.C1C2NC3C(=CC=CC=3)SC=2C=CC=1>[CH3:4][C:3]1([CH3:5])[C:10]2[C:11](=[CH:12][C:6]([O:13][CH3:14])=[C:7]([OH:8])[CH:9]=2)[CH2:1][CH2:2]1
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 460GuaiacolHCID 962WaterHCID 1004Phosphoric AcidHCID 6557Isoprene

生成物 1

HCID 1197896-Methoxy-3,3-dimethylindan-5-ol収率 38.4%

試薬・触媒・溶媒 2

HCID 7108Phenothiazine触媒
HCID 7237
O-Xylene
溶媒

実験手順

449 g of isoprene, stabilized with 1.4 g of phenothiazine, were added dropwise over the course of 6 hours to a solution of 744 g of guaiacol, 76 g of 85% strength phosphoric acid and 6 ml of water in 1.4 liters of xylene at 110° C. To complete the reaction, stirring of the mixture was continued overnight at 110° C. The acid phase was separated off and extracted by shaking with toluene. The combined organic phases were washed until neutral. Fractional distillation gave 443 g of 3,3-dimethyl-5-hydroxy-6-methoxy-indane, boiling point: 145- 46° C/12 mm Hg, melting point 43.5° - 44.5° C. ##STR35##

後処理

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

出典と根拠

ORDレコード
ord-33317a64cd5c417abc04e583d6ee2f58
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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このページの内容参加物実験手順後処理出典と根拠反応ノート