Sodium Hydroxide → HCID 66815743, 화합물

HRID 2367925노트

반응식

HRID 2367925 반응식
[C:1]([O:5][C:6](=[O:29])[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][O:12][C:13]1[CH:14]=[C:15]([C:19]2[N:24]=[C:23]([C:25]([O:27]C)=[O:26])[CH:22]=[CH:21][CH:20]=2)[CH:16]=[CH:17][CH:18]=1)([CH3:4])([CH3:3])[CH3:2].[OH-].[Na+]>CO.O>[C:1]([O:5][C:6](=[O:29])[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][O:12][C:13]1[CH:14]=[C:15]([C:19]2[N:24]=[C:23]([C:25]([OH:27])=[O:26])[CH:22]=[CH:21][CH:20]=2)[CH:16]=[CH:17][CH:18]=1)([CH3:4])([CH3:2])[CH3:3]

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 70206537HCID 70206537, 화합물

생성물 1

HCID 66815743HCID 66815743, 화합물수율 100.1%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

To a solution of compound 8 (840 mg, 2.1 mmol, 1 eq.) in methanol (5 mL) was added NaOH (168 mg, 4.2 mmol, 2 eq.) dissolved in a minimum amount of water. The mixture was stirred at room temperature and monitored by TLC. After completion of the reaction 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 810 mg of crude compound 9, which was used directly in the next step. MS m/z 386 [M+H]+

후처리

  1. customAfter completion of the reaction volatiles
  2. customwere removed in vacuo and ethyl acetate
  3. additionadded
  4. washThe solution was washed with NaH2PO4 buffer (pH 5, 1M) and brine
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-c6d8534402f648179964be1837f7fefb
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08703700B2

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