Hydrogen Bromide → 1-Benzyl-1,4-diazepane

HRID 704389

반응식

HRID 704389 반응식
[CH2:1]([N:8]1[CH2:14][CH2:13][CH2:12][N:11](C(OCC)=O)[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Br>O>[CH2:1]([N:8]1[CH2:14][CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 260Hydrogen BromideHCID 54118699Ethyl 4-benzylhomopiperazine-1-carboxylate

생성물 1

HCID 2283651-Benzyl-1,4-diazepane수율 89.2%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
100 °C

실험 절차

A mixture of 0.85 g of ethyl 4-benzylhomopiperazine-1-carboxylate and 5 ml of 47% hydrobromic acid was heated at 100° C. for 10 hours. After addition of a small amount of water, the reaction mixture was washed with ethyl acetate. The aqueous layer was made alkaline with 30% sodium hydroxide and, after salting out with sodium chloride, extracted with ethyl acetate. The organic layer was washed with saturated aqueous solution of sodium chloride, dried over anhydrous sodium sulfate and concentrated under reduced pressure to give 0.55 g of 1-benzylhomopiperazine.

후처리

  1. washthe reaction mixture was washed with ethyl acetate
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with saturated aqueous solution of sodium chloride
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-2d4cbe5d0ee0429bb7fd06053c051ddc
출처 데이터셋
uspto-grants-1991_01
특허 번호
US04987132

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