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

HRID 1263408ノート

反応式

HRID 1263408 の反応式
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

参加物

7

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 62652Cuprous chloride触媒HCID 962Water溶媒HCID 1004Phosphoric Acid溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-542ff47eaa354c54800ee6ac1c4abec1
出典データセット
uspto-grants-2003_04
特許番号
US06541423B1

反応ノート

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