Sulfuric Acid → HCID 22063473、化合物

HRID 1666164ノート

反応式

HRID 1666164 の反応式
S(=O)(=O)(O)O.[CH2:6]([C:8]1[CH:13]=[CH:12][C:11]([CH2:14][C:15]([CH3:18])(O)[CH3:16])=[CH:10][CH:9]=1)[CH3:7].[C:19](#[N:21])[CH3:20].[OH-:22].[Na+]>C(O)(=O)C>[CH2:6]([C:8]1[CH:13]=[CH:12][C:11]([CH2:14][C:15]([NH:21][C:19](=[O:22])[CH3:20])([CH3:18])[CH3:16])=[CH:10][CH:9]=1)[CH3:7]

参加物

6

反応物 4

HCID 1118Sulfuric AcidHCID 6342AcetonitrileHCID 14798Sodium HydroxideHCID 22063451HCID 22063451、化合物

生成物 1

HCID 22063473HCID 22063473、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

6.2 mL of concentrated sulfuric acid is added dropwise to 15.5 g (87 mmol) of 1-(4-ethylphenyl)-2-methylpropan-2-ol in 4.8 mL (91 mmol) acetonitrile and 15 mL glacial acetic acid within 15 minutes, during which time the temperature rises to 65° C. It is then stirred for one hour, diluted with ice water, and made alkaline with concentrated sodium hydroxide solution. After another 30 minutes' stirring, the solid precipitated is suction filtered and washed with water. The crude product is dissolved in ethyl acetate, dried with sodium sulfate, and evaporated down. The oil remaining is combined with petroleum ether, whereupon a solid is precipitated which is filtered off and dried. Yield: 16.3 g (85%); melting point 90° C.-92° C.

後処理

  1. customrises to 65° C
  2. stirringAfter another 30 minutes' stirring
  3. customthe solid precipitated
  4. filtrationfiltered
  5. washwashed with water
  6. dissolutionThe crude product is dissolved in ethyl acetate
  7. dry with materialdried with sodium sulfate
  8. customevaporated down
  9. customis precipitated which
  10. filtrationis filtered off
  11. customdried

出典と根拠

ORDレコード
ord-3aceaf1e512945c2b2be6bcfa8e83232
出典データセット
uspto-grants-2011_10
特許番号
US08044046B2

反応ノート

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