Hydrochloric Acid → HCID 20088775、化合物

HRID 1975853ノート

反応式

HRID 1975853 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 20088775HCID 20088775、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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 t 0° and 4N HCl (12 mL) is slowly added. The white precipitate is filtered off and washed with H2O. 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.

後処理

  1. temperaturewhile maintaining the temperature at 10°-15° C
  2. temperatureThe reaction mixture is cooled t 0°
  3. filtrationThe white precipitate is filtered off
  4. washwashed with H2O
  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.

出典と根拠

ORDレコード
ord-6fec320536bf4a42b636e73667e40ddf
出典データセット
uspto-grants-1994_02
特許番号
US05288896

反応ノート

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