Lithium Hydroxide → HCID 25744650、化合物

HRID 84191ノート

反応式

HRID 84191 の反応式
[Li+].[OH-].C[O:4][C:5]([C:7]1[CH:8]=[C:9]2[C:13](=[CH:14][CH:15]=1)[N:12]([S:16]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)(=[O:18])=[O:17])[CH2:11][CH2:10]2)=[O:6]>O1CCOCC1>[C:19]1([S:16]([N:12]2[C:13]3[C:9](=[CH:8][C:7]([C:5]([OH:6])=[O:4])=[CH:15][CH:14]=3)[CH2:10][CH2:11]2)(=[O:18])=[O:17])[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1

参加物

4

反応物 2

HCID 3939Lithium HydroxideHCID 31756086Methyl 1-(Phenylsulfonyl)indoline-5-carboxylate

生成物 1

HCID 25744650HCID 25744650、化合物収率 93.4%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
40 °C

実験手順

1M LiOH aqueous solution (2.4 ml, 2.40 mmol) was added to a solution of 11 (0.38 g, 1.20 mmol) in dioxane (15 mL). The reaction mixture was stirred at 40° C. overnight and then was concentrated under reduced pressure. The residue was dissolved in water and concentrated HCl was added up to acidic pH to give the precipitation, which was dried by vacuum to afford 16 (0.34 g). 1H NMR (500 MHz, CD3OD): δ 2.97 (t, J=8.6 Hz, 2H), 3.99 (t, J=8.6 Hz, 2H), 7.51-7.54 (m, 2H), 7.61-7.64 (m, 2H), 7.74 (s, 1H), 7.84-7.88 (m, 3H).

後処理

  1. concentrationwas concentrated under reduced pressure
  2. dissolutionThe residue was dissolved in water
  3. additionconcentrated HCl was added up to acidic pH
  4. customto give
  5. customthe precipitation, which
  6. customwas dried by vacuum

出典と根拠

ORDレコード
ord-b7a24551a1f34319a5084d47e707ac02
出典データセット
uspto-grants-2014_09
特許番号
US08846748B2

反応ノート

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