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Hydrochloric Acid → Methyl 4-Isopropyl-2-hydroxybenzoate

HRID 1787898
ノート
印刷プレビュー

反応式

HRID 1787898 の反応式
[CH:1]([C:4]1[CH:12]=[CH:11][C:7]([C:8]([OH:10])=[O:9])=[C:6]([O:13]COC)[CH:5]=1)([CH3:3])[CH3:2].[C:17](Cl)(=O)C.Cl.C[Si](C=[N+]=[N-])(C)C>C(Cl)Cl.CO.CCCCCC>[CH:1]([C:4]1[CH:12]=[CH:11][C:7]([C:8]([O:10][CH3:17])=[O:9])=[C:6]([OH:13])[CH:5]=1)([CH3:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 6367Acetyl chlorideHCID 167693TrimethylsilyldiazomethaneHCID 685322784-Isopropyl-2-methoxymethoxybenzoic acid

生成物 1

HCID 59745620Methyl 4-Isopropyl-2-hydroxybenzoate

試薬・触媒・溶媒 3

HCID 887Methanol溶媒2 回
HCID 6344
Dichloromethane
溶媒
HCID 8058Hexane溶媒

実験手順

The 4-isopropyl-2-methoxymethoxybenzoic acid (5.3 g, 23.6 mmol) was dissolved in methylene chloride (75 mL) and MeOH (75 mL). Acetyl chloride (1 mL) was added to generate HCl. The reaction mixture was stirred for 2 h. The reaction was washed with water (2×150 mL), dried (MgSO4), and concentrated under vacuum. The crude product was dissolved in methylene chloride (100 mL) and MeOH (30 mL) and to this solution a 2 M hexane solution of (trimethylsilyl)diazomethane (11.8 mL, 23.6 mmol) was added dropwise. After 1 h, the solvent was removed under vacuum, giving the title compound as an oil.

後処理

  1. washThe reaction was washed with water (2×150 mL)
  2. dry with materialdried (MgSO4)
  3. concentrationconcentrated under vacuum
  4. dissolutionThe crude product was dissolved in methylene chloride (100 mL)
  5. waitAfter 1 h
  6. customthe solvent was removed under vacuum

出典と根拠

ORDレコード
ord-34d6ef1d399e470fa61f10610c2eca38
出典データセット
uspto-grants-2009_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07511066B2

反応ノート

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