1-(2-Hydroxyethyl)piperazine → 4-(2-Hydroxyethyl)piperazine-1-carboxamide

HRID 2100425노트

반응식

HRID 2100425 반응식
[OH:1][CH2:2][CH2:3][N:4]1[CH2:9][CH2:8][NH:7][CH2:6][CH2:5]1.C[Si]([N:14]=[C:15]=[O:16])(C)C>C(O)(C)C>[OH:1][CH2:2][CH2:3][N:4]1[CH2:9][CH2:8][N:7]([C:15]([NH2:14])=[O:16])[CH2:6][CH2:5]1

참가 물질

4

반응물 2

HCID 76771-(2-Hydroxyethyl)piperazineHCID 70696Trimethylsilyl isocyanate

생성물 1

HCID 47425144-(2-Hydroxyethyl)piperazine-1-carboxamide수율 88.5%

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

To a stirred solution of 1-(2-hydroxy-ethyl)-piperazine (1.95 g, 15 mmol) in isopropanol (30 mL) at rt was added trimethylsilylisocyanate (2.8 mL, 21 mmol) and the resulting solution stirred overnight before the volatiles were removed in vacuo. The residue was partitioned between CH2Cl2 and water. The aqueous phase was concentrated in vacuo to give 4-(2-hydroxy-ethyl)-piperazine-1-carboxylic acid amide (2.3 g, 88%); 1H-NMR (300 MHz, d6-DMSO) 5.92 (2H, s), 4.40 (1H, t), 3.46-3.52 (2H, m), 3.22-3.34 (4H, m), 2.30-2.39 (6H, m); m/z (ES+) 173 [M+H]+.

후처리

  1. customwere removed in vacuo
  2. customThe residue was partitioned between CH2Cl2 and water
  3. concentrationThe aqueous phase was concentrated in vacuo

출처 및 근거

ORD 기록
ord-b5821917fd8e45ed9f93ad4cebeb7dd4
출처 데이터셋
uspto-grants-2009_08
특허 번호
US07572794B2

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