Hydrochloric Acid → HCID 20088775, 화합물

HRID 275536노트

반응식

HRID 275536 반응식
[BH4-].[Na+].[CH3:3][C:4]([C:7]1[CH:8]=[C:9]([C:18]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[O:19])[CH:10]=[C:11]([C:14]([CH3:17])([CH3:16])[CH3:15])[C:12]=1[OH:13])([CH3:6])[CH3:5].Cl>CCO>[CH3:17][C:14]([C:11]1[CH:10]=[C:9]([CH:18]([C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=2)[OH:19])[CH:8]=[C:7]([C:4]([CH3:3])([CH3:5])[CH3:6])[C:12]=1[OH:13])([CH3:15])[CH3:16]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 1898376(3,5-Di-tert-butyl-4-hydroxyphenyl)(phenyl)methanoneHCID 4311764Sodium borohydride

생성물 1

HCID 20088775HCID 20088775, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Over a 25-minute period NaBH4 (1.89 g, 0.05 mole) is added to a solution of 3.1 g (0.01 mole) of [3,5-bis(1,1-dimethylethyl)-4-hydroxyphenyl]phenylmethanone (C. D. Cook, JOC, 1960, p. 1429) in 50 mL absolute EtOH while maintaining the temperature at 10°-15° C. The reaction mixture is then allowed to come to room temperature for 1.5 hours. The reaction mixture is cooled to 0° and 4N HCl (12 mL) is slowly added. The white precipitate is filtered off and washed with H2. It is taken up in Et2O and washed with saturated NaHCO3. After drying over Na2SO4 the Et2O is evaporated to dryness yielding an analytically pure olive-colored product, 2.9 g (93%), m.p. 117°-119° C.

후처리

  1. temperaturewhile maintaining the temperature at 10°-15° C
  2. temperatureThe reaction mixture is cooled to 0°
  3. filtrationThe white precipitate is filtered off
  4. washwashed with H2
  5. washwashed with saturated NaHCO3
  6. dry with materialAfter drying over Na2SO4 the Et2O
  7. customis evaporated to dryness
  8. customyielding an analytically pure olive-colored product, 2.9 g (93%), m.p. 117°-119° C.

출처 및 근거

ORD 기록
ord-7c84488b7f504cfbbfef1a0914e732d4
출처 데이터셋
uspto-grants-1995_02
특허 번호
US05393923

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