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Ethyl bromoacetate → HCID 12899521, 화합물

HRID 569969
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HRID 569969 반응식
[N:1]1([CH2:7][CH2:8][CH2:9][O:10][C:11]2[CH:20]=[CH:19][CH:18]=[C:17]3[C:12]=2[CH2:13][CH2:14][C:15](=[O:21])[NH:16]3)[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.Br[CH2:23][C:24]([O:26][CH2:27][CH3:28])=[O:25].C(N(CC)CC)C.C(=O)([O-])O.[Na+]>CN(C)C=O>[C:24]([O:26][CH2:27][CH2:28][N:4]1[CH2:5][CH2:6][N:1]([CH2:7][CH2:8][CH2:9][O:10][C:11]2[CH:20]=[CH:19][CH:18]=[C:17]3[C:12]=2[CH2:13][CH2:14][C:15](=[O:21])[NH:16]3)[CH2:2][CH2:3]1)(=[O:25])[CH3:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 7748Ethyl bromoacetateHCID 8471TriethylamineHCID 516892Sodium BicarbonateHCID 14128502HCID 14128502, 화합물

생성물 1

HCID 12899521HCID 12899521, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

20 Grams of 5-(3-piperazinylpropoxy)-3,4-dihydrocarbostyril and 3 ml of ethyl 2-bromoacetate and 1.5 ml of triethylamine are mixed with 20 ml of dimethyl formamide at 50°-60° C. for 8 hours under stirring conditions. The reaction mixture is concentrated under reduced pressure and to the viscous residue thus obtained are added 30 ml of 2% sodium hydrogencarbonate aqueous solution followed by extraction with chloroform. The chloroform layer is washed with water, dried and chloroform is removed by distillation. The residue is purified by silica gel chromatography and recrystallized from isopropanol to obtain 5-{3-[4-(2-acetyloxyethyl)piperazinyl]propoxy}-3,4-dihydrocarbostyril in the form of colorless needle-like crystals with a melting point of 131°-132° C.

후처리

  1. concentrationThe reaction mixture is concentrated under reduced pressure and to the viscous residue
  2. customthus obtained
  3. extractionfollowed by extraction with chloroform
  4. washThe chloroform layer is washed with water
  5. customdried
  6. customchloroform is removed by distillation
  7. customThe residue is purified by silica gel chromatography
  8. customrecrystallized from isopropanol

출처 및 근거

ORD 기록
ord-04326ee31ad5401498f619d3202258ed
출처 데이터셋
uspto-grants-1988_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04734416

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