Lawesson's reagent → [2-(2,6-Dichloro-phenylamino)-phenyl]-acetic acid 4-thiocarbamoyl-phenyl ester

HRID 44162ノート

反応式

HRID 44162 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[NH:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[CH2:16][C:17]([O:19][C:20]1[CH:25]=[CH:24][C:23]([C:26](=O)[NH2:27])=[CH:22][CH:21]=1)=[O:18].COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:38])=CC=1>C1C=CC=CC=1>[C:26]([C:23]1[CH:24]=[CH:25][C:20]([O:19][C:17](=[O:18])[CH2:16][C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[NH:9][C:3]2[C:2]([Cl:1])=[CH:7][CH:6]=[CH:5][C:4]=2[Cl:8])=[CH:21][CH:22]=1)(=[S:38])[NH2:27]

参加物

4

反応物 2

HCID 87949Lawesson's reagentHCID 593455914-Carbamoylphenyl 2-[2-(2,6-dichlorophenylamino)-phenyl]acetate

生成物 1

HCID 25065984[2-(2,6-Dichloro-phenylamino)-phenyl]-acetic acid 4-thiocarbamoyl-phenyl ester収率 91%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

反応条件

温度
50 °C

実験手順

4-Carbamoylphenyl 2-(2-(2,6-dichlorophenylamino)phenyl)acetate (5, 480 mg, 1.14 mmol) and Lawesson reagent (460 mg, 1.14 mmol) were dissolved in 20 ml of anhydrous benzene. The reaction was warmed to 50° C. and stirred for 6 h. The solvent was removed under reduced pressure; the crude residue was purified by silica gel column (dichloromethane/methyl alcohol 9.5/0.5) to furnish the pure compound 6 (446 mg, 91% yield).

後処理

  1. customThe solvent was removed under reduced pressure
  2. customthe crude residue was purified by silica gel column (dichloromethane/methyl alcohol 9.5/0.5)

出典と根拠

ORDレコード
ord-dbcaec4b035a431aa1b6d6e73b38b402
出典データセット
uspto-grants-2013_09
特許番号
US08541398B2

反応ノート

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