Sodium Hydroxide → HCID 66815743、化合物

HRID 2367925ノート

反応式

HRID 2367925 の反応式
[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]

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 70206537HCID 70206537、化合物

生成物 1

HCID 66815743HCID 66815743、化合物収率 100.1%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

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]+

後処理

  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

出典と根拠

ORDレコード
ord-c6d8534402f648179964be1837f7fefb
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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