Triethylamine → N-(2-bromopropionyl)-2-chloro-6-methylbenzylamine

HRID 328625

反応式

HRID 328625 の反応式
[Cl:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([CH3:10])[C:3]=1[CH2:4][NH2:5].C(N(CC)CC)C.[Br:18][CH:19]([CH3:23])[C:20](Br)=[O:21]>C(Cl)CCl>[Br:18][CH:19]([CH3:23])[C:20]([NH:5][CH2:4][C:3]1[C:6]([CH3:10])=[CH:7][CH:8]=[CH:9][C:2]=1[Cl:1])=[O:21]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 79047Propanoyl bromide, 2-bromo-HCID 5217992-Chloro-6-methylbenzylamine

生成物 1

HCID 21442921N-(2-bromopropionyl)-2-chloro-6-methylbenzylamine

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒2 回

反応条件

温度
-35 °C

実験手順

A mixture of 35 parts of 2-chloro-6-methylbenzylamine and 30 parts of triethyl amine in 400 parts of ethylene chloride is stirred and cooled to -35°C. While keeping the temperature between -35° and -20° C., there is added dripwise a solution of 50 parts of 2-bromopropionyl bromide in 160 parts of ethylene chloride. Upon completion, the whole is stirred for one hour at room temperature. The reaction mixture is washed with diluted hydrochloric acid and once with water. The organic phase is dried over magnesium sulfate, filtered and evaporated. The solid residue is crystallized from a mixture of 400 parts of ethanol and 150 parts of water, yielding 40 parts of N-(2-bromopropionyl)-2-chloro-6-methylbenzylamine; mp. 168° -169° C.

後処理

  1. customthe temperature between -35° and -20° C., there
  2. stirringUpon completion, the whole is stirred for one hour at room temperature
  3. washThe reaction mixture is washed with diluted hydrochloric acid and once with water
  4. dry with materialThe organic phase is dried over magnesium sulfate
  5. filtrationfiltered
  6. customevaporated
  7. customThe solid residue is crystallized from a mixture of 400 parts of ethanol and 150 parts of water

出典と根拠

ORDレコード
ord-1b6ce62300c14f95ac4f7a59af9136f3
出典データセット
uspto-grants-1977_04
特許番号
US04017631

関連ノート

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