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Ethyl bromoacetate → HCID 12899521、化合物

HRID 621569
ノート
印刷プレビュー

反応式

HRID 621569 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 7748Ethyl bromoacetateHCID 8471TriethylamineHCID 516892Sodium BicarbonateHCID 14128502HCID 14128502、化合物

生成物 1

HCID 12899521HCID 12899521、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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 hydrogen-carbonate 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.

後処理

  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

出典と根拠

ORDレコード
ord-b9169a7cf2284ad8b782fd9d65f6bd21
出典データセット
uspto-grants-1989_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04824840

反応ノート

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