Hydrochloric Acid → HCID 178447845, 화합물

HRID 465288

반응식

HRID 465288 반응식
[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

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 996PhenolHCID 178447904HCID 178447904, 화합물

생성물 1

HCID 178447845HCID 178447845, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e28bd19730d147eda8d50ce302c07b73
출처 데이터셋
uspto-grants-1992_10
특허 번호
US05152918

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