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Methanol → 4-Benzyloxymethyl-cyclohexanecarboxylic acid methyl ester

HRID 1966073
ノート
印刷プレビュー

反応式

HRID 1966073 の反応式
[CH2:1]([O:8][CH2:9][CH:10]1[CH2:15][CH2:14][CH:13]([CH:16]=[O:17])[CH2:12][CH2:11]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[O-]Cl.[Na+].[CH3:21][OH:22]>C(O)(=O)C>[CH3:21][O:22][C:16]([CH:13]1[CH2:12][CH2:11][CH:10]([CH2:9][O:8][CH2:1][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)[CH2:15][CH2:14]1)=[O:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 887MethanolHCID 186672404-Benzyloxymethyl-cyclohexanecarbaldehydeHCID 23665760Sodium Hypochlorite

生成物 1

HCID 576866884-Benzyloxymethyl-cyclohexanecarboxylic acid methyl ester収率 65%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

To a mixture of (4-benzyloxymethyl-cyclohexyl)-methanol (1.40 g, 6 mmol) in dichloromethane 28 mL is added Dess-Martin periodinate (2.53 g, 6 mmol) at 0° C., and the mixture is stirred for 0.5 hour while warming to room temperature. After addition of saturated aqueous NaHCO3, the mixture is extracted with EtOAc. The combined organic layer after dried over MgSO4 is concentrated to obtain 4-benzyloxymethyl-cyclohexanecarbaldehyde as clear oil (1.07 g, 79%) after purification. 4-Benzyloxymethyl-cyclohexanecarbaldehyde (1.70 g, 2.0 mmol) is dissolved in acetic acid (0.24 mL) and 2 mL of methanol. The reaction mixture is cooled to 0° C. to 5° C. and stirred while 10% NaOCl solution (2.5 mL, 4 mmol) is added dropwise over 20 minutes. The cooling bath is removed, and the mixture is allowed to come to room temperature. After addition of saturated aqueous NaHCO3, the mixture is extracted with EtOAc. The combined organic layer after dried over MgSO4 is concentrated to obtain 4-benzyloxymethyl-cyclohexanecarboxylic acid methyl ester as clear oil (343 mg, 65%) after purification.

後処理

  1. customafter purification
  2. temperatureThe reaction mixture is cooled to 0° C. to 5° C.
  3. additionis added dropwise over 20 minutes
  4. customThe cooling bath is removed
  5. customto come to room temperature
  6. additionAfter addition of saturated aqueous NaHCO3
  7. extractionthe mixture is extracted with EtOAc
  8. dry with materialThe combined organic layer after dried over MgSO4
  9. concentrationis concentrated

出典と根拠

ORDレコード
ord-ea4dabd9267b4104ad71cce2aae9a9bb
出典データセット
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08420641B2

反応ノート

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