4-Toluenesulfonyl chloride → HCID 57799630、化合物

HRID 2100753ノート

反応式

HRID 2100753 の反応式
[OH-].[Na+].[CH3:3][N:4]([CH3:21])[C:5]([C:7]1[CH:8]=[C:9]2[C:13](=[CH:14][C:15]=1[O:16][CH3:17])[CH2:12][C:11](=[N:18]O)[C:10]2=[O:20])=[O:6].C1(C)C=CC(S(Cl)(=O)=[O:29])=CC=1>O>[C:11]([CH2:12][C:13]1[C:9]([C:10]([OH:20])=[O:29])=[CH:8][C:7]([C:5]([N:4]([CH3:3])[CH3:21])=[O:6])=[C:15]([O:16][CH3:17])[CH:14]=1)#[N:18]

参加物

5

反応物 3

HCID 73974-Toluenesulfonyl chlorideHCID 14798Sodium HydroxideHCID 76608766HCID 76608766、化合物

生成物 1

HCID 57799630HCID 57799630、化合物収率 89.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
50 °C

実験手順

To a solution of NaOH (1.6 g, 40.54 mmol) in H2O (30 ml) was added of 2-Hydroxyimino-6-methoxy-3-oxo-indan-5-carboxylic acid dimethylamide (2.8 g, 10.67 mmol). The mixture was heated at 50° C. Then p-Toluenesulfonyl chloride (5.7 g, 30 mmol) was added in portions to the mixture. The mixture was heated at 80° C. for 15 min. After cooling carefully to room temperature, the precipitate (a little) was removed from the mixture. Mother liquid was acidified by concentrated HCl to PH=3-4 and the precipitate was collected and dried to give product (2.5 g, 89.28%). LC-MS: m/e 261 (M−1).

後処理

  1. temperatureThe mixture was heated at 80° C. for 15 min
  2. temperatureAfter cooling carefully to room temperature
  3. customthe precipitate (a little) was removed from the mixture
  4. customthe precipitate was collected
  5. customdried

出典と根拠

ORDレコード
ord-1b188bf0cba84642bf6881c0a01a12ba
出典データセット
uspto-grants-2009_08
特許番号
US07572809B2

反応ノート

読み込み中…