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Triethylamine → 1-[4-(2-Methylacryloyl)piperazin-1-yl]butane-1,3-dione

HRID 905103
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HRID 905103 반응식
Br.[C:2]([N:8]1[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1)(=[O:7])[CH2:3][C:4]([CH3:6])=[O:5].C(N(CC)CC)C.[C:21](Cl)(=[O:25])[C:22]([CH3:24])=[CH2:23]>CN(C)C=O.CC1C=CC(S(NC2C=CC(NC3C=CC=CC=3)=CC=2)(=O)=O)=CC=1>[C:2]([N:8]1[CH2:13][CH2:12][N:11]([C:21](=[O:25])[C:22]([CH3:24])=[CH2:23])[CH2:10][CH2:9]1)(=[O:7])[CH2:3][C:4]([CH3:6])=[O:5]
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참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 13528Methacryloyl chlorideHCID 204670771-Acetoacetylpiperazine hydrobromide

생성물 1

HCID 226089801-[4-(2-Methylacryloyl)piperazin-1-yl]butane-1,3-dione수율 56%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매
HCID 66856
Benzenesulfonamide, 4-methyl-N-[4-(phenylamino)phenyl]-
용매

실험 절차

Crude 1-acetoacetylpiperazine hydrobromide (50 g, 0.2 mole) was dissolved in N,N-dimethylformamide (300 ml) with Aranox® (50 mg) (available from U.S. Rubber Co.). Triethylamine (50 g, 0.5 mole) was added at 0° C., followed immediately by the dropwise addition of methacryloyl chloride (20.8 g, 0.2 mole) at 0° C. The reaction solution was then allowed to reach 20° C. over a 20 hour period. The reaction solution was filtered and the solvent was removed at low vacuum. The residue was distilled to give 4-acetoacetyl-1-methacryloylpiperazine (b.p.=110°-129° C./10-8μ) at a yield of 56%.

후처리

  1. filtrationThe reaction solution was filtered
  2. customthe solvent was removed at low vacuum
  3. distillationThe residue was distilled

출처 및 근거

ORD 기록
ord-3d678fd9b8494b5eb164cd19ab180f2f
출처 데이터셋
uspto-grants-1983_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04421915

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