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Methanol → HCID 118061920、化合物

HRID 920757
ノート
印刷プレビュー

反応式

HRID 920757 の反応式
[F:1][CH:2]([F:13])[O:3][CH2:4][C@@H:5]1[CH2:8][CH2:7][C@H:6]1[C:9]([O:11]C)=[O:10].CO.[OH-].[Na+]>O>[F:1][CH:2]([F:13])[O:3][CH2:4][C@@H:5]1[CH2:8][CH2:7][C@H:6]1[C:9]([OH:11])=[O:10]
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 14798Sodium HydroxideHCID 118069263HCID 118069263、化合物

生成物 1

HCID 118061920HCID 118061920、化合物収率 86.2%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a solution of Intermediate 241A (100 mg, 0.515 mmol) in a 1:0.3:1THF:MeOH:water was added NaOH (41.2 mg, 1.030 mmol) and the resulting solution was stirred at RT for 12 h. The volatiles were removed under reduced pressure and the aqueous layer was washed with ethyl acetate. The pH of the aqueous layer was adjusted to 4 by adding an aqueous solution of 1.5 N HCl and extracted with ethyl acetate (3×10 mL) The combined organic layer was dried over Na2SO4 and evaporated under vacuum to afford Intermediate 241B as yellow sticky liquid (80 mg, 86%). 1H NMR (300 MHz, DMSO-d6) δ ppm 12.10 (s, 1H), 6.35-6.95 (m, 1H), 3.74-3.89 (m, 2H), 2.85 (q, J=8.70 Hz, 1H) 2.63-2.77 (m, 1H) 1.95-2.10 (m, 4H).

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. customThe volatiles were removed under reduced pressure
  2. washthe aqueous layer was washed with ethyl acetate
  3. additionby adding an aqueous solution of 1.5 N HCl
  4. extractionextracted with ethyl acetate (3×10 mL) The combined organic layer
  5. dry with materialwas dried over Na2SO4
  6. customevaporated under vacuum

出典と根拠

ORDレコード
ord-006b4165109f41cc89a8928e34e29596
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09273058B2

反応ノート

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