Triethylamine → Benzophenone hydrochloride

HRID 1973527

반응식

HRID 1973527 반응식
BrCC(N[C:6]1[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][C:7]=1[C:8]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)=[O:9])=O.Cl.NC(C)CO.C(N(CC)CC)C>C(O)C>[ClH:20].[C:8]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)(=[O:9])[C:7]1[CH:16]=[CH:17][CH:18]=[CH:19][CH:6]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 1107982-Aminopropanol hydrochlorideHCID 122906N-(2-benzoyl-4-chlorophenyl)-2-bromoacetamide

생성물 1

HCID 19775659Benzophenone hydrochloride

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 79.4 g. (225 mmole) of 2-(2-bromoacetamido)-5-chlorobenzophenone, 25 g. of 2-aminopropanol hydrochloride, 95 ml. of triethylamine and 500 ml. of ethanol was stirred overnight at room temperature, and then at reflux for 5 hours. The solution was concentrated under reduced pressure to a residue which was partitioned between ether and water. The organic layer was washed with water, dried and treated with hydrogen chloride to give 18 g. of a colorless solid. Recrystallizations from ethanol-ether gave prisms of 5-chloro-2-[2-hydroxy-2-propylamino)acetimido]-benzophenone, hydrochloride, m.p. 183°-186°.

후처리

  1. additionA mixture of 79.4 g
  2. temperatureat reflux for 5 hours
  3. concentrationThe solution was concentrated under reduced pressure to a residue which
  4. customwas partitioned between ether and water
  5. washThe organic layer was washed with water
  6. customdried
  7. additiontreated with hydrogen chloride
  8. customto give 18 g
  9. customRecrystallizations from ethanol-ether

출처 및 근거

ORD 기록
ord-6996254ade3a4b7ca930a84e796b972c
출처 데이터셋
uspto-grants-1976_12
특허 번호
US03997591

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