Methanol → HCID 66815646, 화합물

HRID 2367923노트

반응식

HRID 2367923 반응식
[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]

참가 물질

4

반응물 2

HCID 887MethanolHCID 67773395HCID 67773395, 화합물

생성물 1

HCID 66815646HCID 66815646, 화합물

시약·촉매·용매 1

HCID 21901998Ethyl acetate hexane acetic acid용매

실험 절차

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]+

후처리

  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

출처 및 근거

ORD 기록
ord-8a3ab6d0e0ef45a09927719a63c9fab4
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08703700B2

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