Hydrochloric Acid → HCID 178447845、化合物

HRID 465288

反応式

HRID 465288 の反応式
[CH2:1]([C@H:4]1[CH2:9][CH2:8][C@H:7]([CH:10]2[CH2:15][CH2:14][C:13](=[O:16])[CH2:12][CH2:11]2)[CH2:6][CH2:5]1)[CH2:2][CH3:3].[C:17]1([OH:23])[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.Cl.O>C1(C)C=CC=CC=1>[OH:16][C:13]1[CH:14]=[CH:15][C:10]([C:7]2([C:20]3[CH:21]=[CH:22][C:17]([OH:23])=[CH:18][CH:19]=3)[CH2:6][CH2:5][CH:4]([C@H:1]3[CH2:3][CH2:2][C@H:1]([CH2:4][CH2:5][CH3:6])[CH2:3][CH2:2]3)[CH2:9][CH2:8]2)=[CH:11][CH:12]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 996PhenolHCID 178447904HCID 178447904、化合物

生成物 1

HCID 178447845HCID 178447845、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

4-(Trans-4-n-propylcyclohexyl)cyclohexanone (449 g), phenol (756 g) and CaCl (446 g) were mixed, followed by gradually dropwise adding conc. hydrochloric acid (335 ml) with vigorous stirring at room temperature, further agitating the mixture for 30 minutes after completion of the dropwise addition, allowing the resulting material to stand at room temperature, further for 50 hours, adding hot water (2 l) and toluene (3 l), heating the mixture, cooling, filtering off crystals, washing the crystals with water and then with toluene, drying the crystals and recrystallizing from tetrahydrofuran solvent to obtain white crystals of 1,1-bis(4-hydroxyphenyl)-4-(trans-4-n-propylcyclohexyl)cyclohexane as a diol compound of the present invention (436 g). M.P.: 222.0°-222.8° C.

後処理

  1. stirringfurther agitating the mixture for 30 minutes
  2. additionafter completion of the dropwise addition
  3. temperatureheating the mixture
  4. temperaturecooling
  5. filtrationfiltering off crystals
  6. washwashing the crystals with water
  7. dry with materialwith toluene, drying the crystals
  8. customrecrystallizing from tetrahydrofuran solvent

出典と根拠

ORDレコード
ord-e28bd19730d147eda8d50ce302c07b73
出典データセット
uspto-grants-1992_10
特許番号
US05152918

関連ノート

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