2-Chloroethyl Isothiocyanate → 2-Chloro-4-(2-thiazolinylamino)benzoic acid methyl ester

HRID 24715

反応式

HRID 24715 の反応式
[CH3:1][O:2][C:3](=[O:12])[C:4]1[CH:9]=[CH:8][C:7]([NH2:10])=[CH:6][C:5]=1[Cl:11].Cl[CH2:14][CH2:15][N:16]=[C:17]=[S:18]>C1COCC1>[CH3:1][O:2][C:3](=[O:12])[C:4]1[CH:9]=[CH:8][C:7]([NH:10][C:17]2[S:18][CH2:14][CH2:15][N:16]=2)=[CH:6][C:5]=1[Cl:11]

参加物

4

反応物 2

HCID 1386612-Chloroethyl IsothiocyanateHCID 11839197Methyl 4-Amino-2-chlorobenzoate

生成物 1

HCID 695646282-Chloro-4-(2-thiazolinylamino)benzoic acid methyl ester

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 4-amino-2-chlorobenzoic acid methyl ester (0.5 g) and 2-chloroethylisothiocyanate (0.26 mL) in THF (20 mL) was refluxed for 24 h. THF was distilled and the residue was purified by column chromatography (silica gel: eluent: hexane/EtOAc 3:1-1:1) to yield 2-chloro-4-(2-thiazolinylamino)benzoic acid methyl ester (74 mg). ESMS: m/z 271 (MH+).

後処理

  1. temperaturewas refluxed for 24 h
  2. distillationTHF was distilled
  3. customthe residue was purified by column chromatography (silica gel: eluent: hexane/EtOAc 3:1-1:1)

出典と根拠

ORDレコード
ord-2a25a18e5f0c4c359bac4a1888fb1f0e
出典データセット
uspto-grants-2005_02
特許番号
US06855843B2

関連ノート

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