Dichloromethane → HCID 57378117、化合物

HRID 511907ノート

反応式

HRID 511907 の反応式
C(N(CC)CC)C.[C:8]([N:15]1[CH:19]=[CH:18]N=C1)(N1C=CN=C1)=[S:9].C(Cl)Cl.NC1C=[CH:31][C:27]([C:28]([OH:30])=[O:29])=[C:26]([N+:33]([O-:35])=[O:34])[CH:25]=1>C(OCC)(=O)C>[N:15]([C:19]1[CH:18]=[CH:31][C:27]([C:28]([OH:30])=[O:29])=[C:26]([N+:33]([O-:35])=[O:34])[CH:25]=1)=[C:8]=[S:9]

参加物

6

反応物 4

HCID 6344DichloromethaneHCID 8471TriethylamineHCID 802641,1'-ThiocarbonyldiimidazoleHCID 2357134-Amino-2-nitrobenzoic Acid

生成物 1

HCID 57378117HCID 57378117、化合物収率 89%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

Triethylamine (55.8 μL, 0.4 mmol) and thiocarbonyldiimidazole (46.3 mg, 0.26 mmol) were added to a methylene chloride solution (0.4 mL) of 4-amino-2-nitrobenzoic acid (36.4 mg, 0.2 mmol) at room temperature, followed by stirring at room temperature for 10 minutes. The reaction mixture was dissolved in ethyl acetate and washed with 1 M hydrochloric acid, the organic layer was separated, and then the organic layer was dried over magnesium sulfate. Thereafter, filtration and concentration under reduced pressure to dryness were carried out to obtain 4-isothiocyanato-2-nitrobenzoic acid as a colorless solid (40 mg, yield: 89%, HPLC purity: 96.4%)

後処理

  1. washwashed with 1 M hydrochloric acid
  2. customthe organic layer was separated
  3. dry with materialthe organic layer was dried over magnesium sulfate
  4. filtrationThereafter, filtration and concentration under reduced pressure to dryness

出典と根拠

ORDレコード
ord-3ec28024c9bd4081b8104eea24de2c4b
出典データセット
uspto-grants-2015_08
特許番号
US09102602B2

反応ノート

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