Ethanol → Benzothiazole, 5,6-dimethoxy-2-methyl-

HRID 1881174노트

반응식

HRID 1881174 반응식
Br[C:2]1[CH:7]=[C:6]([O:8][CH3:9])[C:5]([O:10][CH3:11])=[CH:4][C:3]=1[N+:12]([O-])=O.[S-2:15].[Na+].[Na+].[S].[CH2:19](O)[CH3:20]>>[CH3:11][O:10][C:5]1[C:6]([O:8][CH3:9])=[CH:7][C:2]2[S:15][C:19]([CH3:20])=[N:12][C:3]=2[CH:4]=1

참가 물질

5

반응물 4

HCID 702Ethanol2회HCID 14804Sodium SulfideHCID 1709684-Bromo-5-nitroveratroleHCID 5362487Sulfur

생성물 1

HCID 112829Benzothiazole, 5,6-dimethoxy-2-methyl-

실험 절차

1-Bromo-4,5-dimethoxy-2-nitro-benzene (10 g) was suspended into ethanol (50 ml). To the reaction mixture was added the suspension of sodium sulfide (5 g) and sulfur (0.65 g) in ethanol (12 ml). The reaction mixture was refluxed 1.5 hour and then the resultant solid was filtered and washed with hot water and ethanol. The dry solid was slurried with acetic acid (60 ml) and acetanhydridi (35 ml). To the suspension was gradually added zinc (16.6 g) and the suspension was stirred at room temperature for 15 min before filtering off. The residue was evaporated to dryness. The product was purified by column chromatography using toluene-ethyl acetate-acetic acid 8:1:1 as the eluent.

후처리

  1. additionTo the reaction mixture was added
  2. temperatureThe reaction mixture was refluxed 1.5 hour
  3. filtrationthe resultant solid was filtered
  4. washwashed with hot water and ethanol
  5. filtrationbefore filtering off
  6. customThe residue was evaporated to dryness
  7. customThe product was purified by column chromatography

출처 및 근거

ORD 기록
ord-e2b8445e6e684076841356a2e6169893
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08318785B2

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