4-Nitrobenzoyl chloride → 2-(4-Nitrophenyl)Benzo[D]Thiazole

HRID 898079ノート

反応式

HRID 898079 の反応式
[N+:1]([C:4]1[CH:12]=[CH:11][C:7]([C:8](Cl)=O)=[CH:6][CH:5]=1)([O-:3])=[O:2].[NH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=1[SH:20]>C1C=CC=CC=1>[N+:1]([C:4]1[CH:12]=[CH:11][C:7]([C:8]2[S:20][C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=3[N:13]=2)=[CH:6][CH:5]=1)([O-:3])=[O:2]

参加物

4

反応物 2

HCID 85024-Nitrobenzoyl chlorideHCID 87132-Aminothiophenol

生成物 1

HCID 8275002-(4-Nitrophenyl)Benzo[D]Thiazole収率 73.2%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

A solution of 4-nitrobenzoyl chloride (1.49 g, 8.0 mmol) in benzene anhydrous, 10 mL) was added dropwise to 2-aminothiophenol (1.0 g, 8.0 mmol in 10 ml of benzene) at room temperature. The reaction mixture was allowed to stir for 16 hr. The reaction was quenched with water (20 mL). The aqueous layer was separated and extracted with ethyl acetate (3×10 ml). The combined organic layers were dried and evaporated. The crude product was purified with flush column, (hexane:ethyl acetate=85:15) to give 1.5 g (73.2%) of product as light yellow solid.

後処理

  1. customThe reaction was quenched with water (20 mL)
  2. customThe aqueous layer was separated
  3. extractionextracted with ethyl acetate (3×10 ml)
  4. customThe combined organic layers were dried
  5. customevaporated
  6. customThe crude product was purified
  7. customwith flush column, (hexane:ethyl acetate=85:15)

出典と根拠

ORDレコード
ord-5604215748e24f859d16b9a30f4d0eab
出典データセット
uspto-grants-2008_04
特許番号
US07351401B2

反応ノート

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