Ethyl bromoacetate → HCID 54510282、化合物

HRID 2296493ノート

反応式

HRID 2296493 の反応式
[OH:1][C:2]1[C:3]([Br:13])=[C:4]([C:8]([Br:12])=[CH:9][C:10]=1[Br:11])[C:5]([NH2:7])=[O:6].[Na].Br[CH2:16][C:17]([O:19][CH2:20]C)=[O:18]>CO>[CH3:20][O:19][C:17](=[O:18])[CH2:16][O:1][C:2]1[C:10]([Br:11])=[CH:9][C:8]([Br:12])=[C:4]([C:5](=[O:6])[NH2:7])[C:3]=1[Br:13]

参加物

5

反応物 3

HCID 7748Ethyl bromoacetateHCID 5360545SodiumHCID 19848363HCID 19848363、化合物

生成物 1

HCID 54510282HCID 54510282、化合物収率 88%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

35.5 g (95 mmol) of 3-hydroxy-2,4,6-tribromobenzamide is suspended in 150 ml of methanol and dissolved by adding 2.18 g (95 mmol) of sodium. The mixture is combined with 17.5 g (104 mmol) of ethyl bromoacetate and maintained under reflux for three hours. After several hours of agitation, the crystallized product is vacuum-filtered, washed with a small amount of ice-cold methanol, and dried at 60° C., thus obtaining 37.2 g (88% of theory) of 3-carbamoyl-2,4,6-tribromophenoxyacetic acid methyl ester, mp 231°-233° C.

後処理

  1. dissolutiondissolved
  2. temperaturemaintained
  3. temperatureunder reflux for three hours
  4. waitAfter several hours of agitation
  5. filtrationthe crystallized product is vacuum-filtered
  6. washwashed with a small amount of ice-cold methanol
  7. customdried at 60° C.

出典と根拠

ORDレコード
ord-d6c31396983b4018a1a74afab4206ef2
出典データセット
uspto-grants-1984_01
特許番号
US04429152

反応ノート

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