Hydrochloric Acid → Methyl 2-chloro-4-methylbenzo[d]thiazole-5-carboxylate

HRID 1263408노트

반응식

HRID 1263408 반응식
N([O-])=O.[Na+].N[C:6]1[S:7][C:8]2[CH:14]=[CH:13][C:12]([C:15]([O:17][CH3:18])=[O:16])=[C:11]([CH3:19])[C:9]=2[N:10]=1.[ClH:20]>O.P(=O)(O)(O)O.Cl[Cu]>[Cl:20][C:6]1[S:7][C:8]2[CH:14]=[CH:13][C:12]([C:15]([O:17][CH3:18])=[O:16])=[C:11]([CH3:19])[C:9]=2[N:10]=1

참가 물질

7

반응물 3

HCID 313Hydrochloric AcidHCID 22390084Methyl 2-amino-4-methylbenzo[d]thiazole-5-carboxylateHCID 23668193Sodium Nitrite

생성물 1

HCID 22390080Methyl 2-chloro-4-methylbenzo[d]thiazole-5-carboxylate

시약·촉매·용매 3

HCID 62652Cuprous chloride촉매HCID 962Water용매HCID 1004Phosphoric Acid용매

반응 조건

온도
100 °C

실험 절차

At −8° C., a solution of 9.3 g of NaNO2 (0.14 mol) in 10 ml of water was added dropwise to a solution of 5 g of methyl 2-amino-4-methylbenzothiazole-5-carboxylate (0.02 mol) in 150 ml of phosphoric acid. At 5° C., a solution of 3 g of CuCl and 12 ml of conc. HCl was then added dropwise. The reaction mixture was heated to 100° C. After cooling, the residue was filtered off with suction, washed with water and dried. The product was purified by silica gel column chromatography.

후처리

  1. temperatureAfter cooling
  2. filtrationthe residue was filtered off with suction
  3. washwashed with water
  4. customdried
  5. customThe product was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-542ff47eaa354c54800ee6ac1c4abec1
출처 데이터셋
uspto-grants-2003_04
특허 번호
US06541423B1

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