3-Methyl-3-buten-1-ol → HCID 23289305, 화합물

HRID 366465

반응식

HRID 366465 반응식
[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

참가 물질

6

반응물 4

HCID 129883-Methyl-3-buten-1-olHCID 14798Sodium HydroxideHCID 70297m-Chloroperbenzoic acidHCID 23289308HCID 23289308, 화합물

생성물 1

HCID 23289305HCID 23289305, 화합물수율 63%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9f5820d817c84634b329b7474379812f
출처 데이터셋
uspto-grants-2000_10
특허 번호
US06130217

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