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Water → 1-(1,3-Benzodioxol-5-YL)-3-(4-phenyl-1-piperazinyl)-1-propanone

HRID 1788670
ノート
印刷プレビュー

反応式

HRID 1788670 の反応式
Cl[CH2:2][CH2:3][C:4]([C:6]1[CH:14]=[CH:13][C:9]2[O:10][CH2:11][O:12][C:8]=2[CH:7]=1)=[O:5].[C:15]1([N:21]2[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]2)[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.C(N(CC)CC)C.O>CN(C=O)C>[C:15]1([N:21]2[CH2:26][CH2:25][N:24]([CH2:2][CH2:3][C:4]([C:6]3[CH:14]=[CH:13][C:9]4[O:10][CH2:11][O:12][C:8]=4[CH:7]=3)=[O:5])[CH2:23][CH2:22]2)[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1
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 962WaterHCID 70961-PhenylpiperazineHCID 8471TriethylamineHCID 2705941-(1,3-Benzodioxol-5-yl)-3-chloropropan-1-one

生成物 1

HCID 6762451-(1,3-Benzodioxol-5-YL)-3-(4-phenyl-1-piperazinyl)-1-propanone収率 84%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide
溶媒

実験手順

5-(3-Chloropropionyl)-1,3-benzodioxole (3 g) and N-phenylpiperazine (2.4 g) were dissolved in DMF (20 ml), triethylamine (1.7 g) was then added and the mixture was stirred for 10 hours at room temperature. After completion of the reaction, the reaction mixture was poured into water and extracted with ethyl acetate. The extract was dried over anhydrous sodium sulfate and the solvent was distilled off. The residue was crystallized from methanol and the resulting crystals were recrystallized from ethanol to give 5-[3-(4-phenyl-1-piperazinyl)propionyl]-1,3-benzodioxole (4.0 g, 84% yield). The characteristics of this compound are shown in Table 3 as Compound 47.

後処理

  1. customAfter completion of the reaction
  2. extractionextracted with ethyl acetate
  3. dry with materialThe extract was dried over anhydrous sodium sulfate
  4. distillationthe solvent was distilled off
  5. customThe residue was crystallized from methanol
  6. customthe resulting crystals were recrystallized from ethanol

出典と根拠

ORDレコード
ord-117875f1ff4345cb90ccb856fbe3a579
出典データセット
uspto-grants-1987_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04684651

反応ノート

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