Sodium Hydroxide → BPTMC phenol

HRID 488544

반응식

HRID 488544 반응식
[OH-].[Na+].[CH3:3][CH:4]1[CH2:9][C:8]([C:17]2[CH:22]=[CH:21][C:20]([OH:23])=[CH:19][CH:18]=2)([C:10]2[CH:15]=[CH:14][C:13]([OH:16])=[CH:12][CH:11]=2)[CH2:7][C:6]([CH3:25])([CH3:24])[CH2:5]1>>[CH3:3][CH:4]1[CH2:9][C:8]([C:10]2[CH:11]=[CH:12][C:13]([OH:16])=[CH:14][CH:15]=2)([C:17]2[CH:22]=[CH:21][C:20]([OH:23])=[CH:19][CH:18]=2)[CH2:7][C:6]([CH3:24])([CH3:25])[CH2:5]1.[C:13]1([OH:16])[CH:14]=[CH:15][CH:10]=[CH:11][CH:12]=1

참가 물질

3

반응물 2

HCID 14798Sodium HydroxideHCID 41340354,4'-(3,3,5-Trimethylcyclohexylidene)bis(phenol)

생성물 1

HCID 70193612BPTMC phenol

반응 조건

온도
95 °C

실험 절차

The reaction was carried out as described in Reference Example 1 and the reaction mixture obtained after completion of the reaction was neutralized at pH 6.5 by adding an 18% aqueous sodium hydroxide solution while maintaining the temperature at 40–50° C. Next, the temperature of the reaction mixture thus neutralized was raised to 95° C. to dissolve the generated BPTMC adduct crystals, after which the resulting water phase was removed by separation, and the temperature of the oil phase obtained was rapidly lowered to 40° C. with a temperature gradient of about 20° C./hour to crystallize the BPTMC-phenol adduct, and the crystals of the BPTMC-phenol adduct were obtained by centrifugal filtration.

후처리

  1. customthe reaction mixture obtained after completion of the reaction
  2. temperaturewhile maintaining the temperature at 40–50° C
  3. customafter which the resulting water phase was removed by separation
  4. customthe temperature of the oil phase obtained
  5. customwas rapidly lowered to 40° C. with a temperature gradient of about 20° C./hour
  6. customto crystallize the BPTMC-phenol adduct

출처 및 근거

ORD 기록
ord-a2c9374e998f4d58b99eb5befbaf40f1
출처 데이터셋
uspto-grants-2005_12
특허 번호
US06972344B2

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