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

HRID 328625

반응식

HRID 328625 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매2회

반응 조건

온도
-35 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1b6ce62300c14f95ac4f7a59af9136f3
출처 데이터셋
uspto-grants-1977_04
특허 번호
US04017631

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