Methanol → HCID 66815646、化合物

HRID 2367923ノート

反応式

HRID 2367923 の反応式
[C:1]([O:5][C:6](=[O:27])[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][O:12][C:13]1[CH:14]=[CH:15][CH:16]=[C:17]2[C:22]=1[N:21]=[C:20]([C:23]([O:25]C)=[O:24])[CH:19]=[CH:18]2)([CH3:4])([CH3:3])[CH3:2].CO>C(OCC)(=O)C.CCCCCC.C(O)(=O)C>[C:1]([O:5][C:6](=[O:27])[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][O:12][C:13]1[CH:14]=[CH:15][CH:16]=[C:17]2[C:22]=1[N:21]=[C:20]([C:23]([OH:25])=[O:24])[CH:19]=[CH:18]2)([CH3:4])([CH3:2])[CH3:3]

参加物

4

反応物 2

HCID 887MethanolHCID 67773395HCID 67773395、化合物

生成物 1

HCID 66815646HCID 66815646、化合物

試薬・触媒・溶媒 1

HCID 21901998Ethyl acetate hexane acetic acid溶媒

実験手順

To a solution of compound 1 (540 mg, 1.45 mmol, 1 eq.) in MeOH (3 mL) NaOH (116 mg, 2.9 mmol, 2 eq.) was added as, a concentrated aqueous solution, and the mixture was stirred at room temperature. The reaction was monitored by TLC (ethyl acetate/hexane/acetic acid, 1:1:0.01). Upon completion the volatiles were removed in vacuo and ethyl acetate added. The solution was washed with NaH2PO4 buffer (pH 5, 1M) and brine, dried over Na2SO4, and concentrated in vacuo to give 446 mg of crude 2, which was used directly in the next step. MS m/z 360 [M−H]+

後処理

  1. customUpon completion the volatiles were removed in vacuo and ethyl acetate
  2. additionadded
  3. washThe solution was washed with NaH2PO4 buffer (pH 5, 1M) and brine
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated in vacuo
  6. customto give 446 mg of crude 2, which

出典と根拠

ORDレコード
ord-8a3ab6d0e0ef45a09927719a63c9fab4
出典データセット
uspto-grants-2014_04
特許番号
US08703700B2

反応ノート

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