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Hydrochloric Acid → 2-Chloro-4,6-difluorobenzothiazole

HRID 907707
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HRID 907707 반응식
N(OCCC(C)C)=O.[F:9][C:10]1[C:15]2[N:16]=[C:17](N)[S:18][C:14]=2[CH:13]=[C:12]([F:20])[CH:11]=1.[ClH:21]>C(#N)C.[Cu](Cl)Cl>[Cl:21][C:17]1[S:18][C:14]2[CH:13]=[C:12]([F:20])[CH:11]=[C:10]([F:9])[C:15]=2[N:16]=1
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참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 8053Isoamyl NitriteHCID 7374064,6-Difluoro-1,3-benzothiazol-2-amine

생성물 1

HCID 20498832-Chloro-4,6-difluorobenzothiazole수율 99%

시약·촉매·용매 2

HCID 24014Cupric Chloride촉매HCID 6342Acetonitrile용매

실험 절차

To a solution containing copper chloride (II) (0.87 g, 6.45 mmol) and tri(ethylene glycol) dimethyl ether (3 mL) in acetonitrile (50 mL) was added isoamyl nitrite (0.94 g, 8.06 mmol), and the reaction mixture was stirred at rt for 30 minutes. To this suspension was added dropwise a solution of 4,6-difluoro-1,3-benzothiazol-2-amine (1.0 g, 5.37 mmol) in tri(ethylene glycol) dimethyl ether (5 mL). The reaction mixture was stirred at rt for 10 minutes, and then heated at 50° C. for 2.5 h. The reaction mixture was cooled to rt, and then poured cautiously into cold aqueous 6 M HCl (200 mL). The solution was extracted with EtOAc. The organic layer was washed with HCl (1.0 M), water and brine, filtered and concentrated down to afford 2-chloro-4,6-difluoro-1,3-benzothiazole (1.1 g, 99%). 1H NMR (400 MHz, DMSO-d6) 7.05 (m, 1H), 7.36 (m, 1H).

후처리

  1. stirringThe reaction mixture was stirred at rt for 10 minutes
  2. temperatureheated at 50° C. for 2.5 h
  3. temperatureThe reaction mixture was cooled to rt
  4. extractionThe solution was extracted with EtOAc
  5. washThe organic layer was washed with HCl (1.0 M), water and brine
  6. filtrationfiltered
  7. concentrationconcentrated down

출처 및 근거

ORD 기록
ord-29bbf8865b504dceacd13da25e81dc7a
출처 데이터셋
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08013166B2

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