Hydrochloric Acid → [(4-Chloro-3-fluorophenyl)carbamoyl]formic acid

HRID 626610ノート

反応式

HRID 626610 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9](=[O:15])[C:10]([O:12]CC)=[O:11])=[CH:4][C:3]=1[F:16].[OH-].[Na+].CCO.Cl>O>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9](=[O:15])[C:10]([OH:12])=[O:11])=[CH:4][C:3]=1[F:16]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 14798Sodium HydroxideHCID 57523348Ethyl 2-(4-chloro-3-fluorophenylamino)-2-oxoacetate

生成物 1

HCID 22934746[(4-Chloro-3-fluorophenyl)carbamoyl]formic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Ethyl 2-(4-chloro-3-fluorophenylamino)-2-oxoacetate (4.18 g, 0.017 mol) to a solution of NaOH (1.361 g, 0.0340 mol) in mixture 50 ml EtOH and 50 ml water was added and the resulting mixture was stirred at RT for 6 h. The mixture was acidified with 2N HCl to pH 4-5 at 0° C. The precipitate was filtered, washed with water and dried on the air to afford 2-(4-chloro-3-fluorophenylamino)-2-oxoacetic acid (3′) (2 g, 55.2%) as a white solid. LC-MS (APCI+) m/z: calcd for C8H5ClFNO3: 216.99. found: 217 (M+H+).

後処理

  1. filtrationThe precipitate was filtered
  2. washwashed with water
  3. customdried on the air

出典と根拠

ORDレコード
ord-d62b37fbabb94ecd94e6daf23d99eef6
出典データセット
uspto-grants-2016_04
特許番号
US09309237B2

反応ノート

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