3-Methyl-3-buten-1-ol → HCID 23289305、化合物

HRID 366465

反応式

HRID 366465 の反応式
[CH3:1][C:2]1[S:3][C:4]2[C:10]([OH:11])=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=1.CC(=C)CCO.Cl[C:19]1C=C[CH:22]=[C:21]([C:25]([O:27]O)=O)[CH:20]=1.[OH-].[Na+]>C(Cl)Cl>[CH3:1][C:2]1[S:3][C:4]2[C:10]([O:11][CH2:19][CH2:20][C:21]3([CH3:22])[CH2:25][O:27]3)=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=1

参加物

6

反応物 4

HCID 129883-Methyl-3-buten-1-olHCID 14798Sodium HydroxideHCID 70297m-Chloroperbenzoic acidHCID 23289308HCID 23289308、化合物

生成物 1

HCID 23289305HCID 23289305、化合物収率 63%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

2-Methyl-7-hydroxybenzothiazoie was alkylated with 3-methyl-3-buten-1-ol according to Method VI. The product of this alkylation (0.30 g, 1.28 mmol) was dissolved in CH2Cl2 at about 0° C. to which was then added a solution of m-chloroperbenzoic acid (0.95 g, 5.53 mmol) in CH2Cl2. The reaction was allowed to warm to room temperature and after about 0.5 h the reaction was complete. 1N NaOH was added, the layers separated and the organic layer was washed with additional 1N NaOH and H2O. The organic layer was then dried over MgSO4 and the solvent was removed by rotary evaporation to give the title compound (0.20 g, 63%) as a yellow oil which was used in subsequent reactions without further purification.

後処理

  1. customthe layers separated
  2. washthe organic layer was washed with additional 1N NaOH and H2O
  3. dry with materialThe organic layer was then dried over MgSO4
  4. customthe solvent was removed by rotary evaporation

出典と根拠

ORDレコード
ord-9f5820d817c84634b329b7474379812f
出典データセット
uspto-grants-2000_10
特許番号
US06130217

関連ノート

読み込み中…