홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Potassium Carbonate → 4'-Acetamido-2'-benzyloxy-2-[4-(benzyloxycarbonyl)piperazin-1-yl]acetophenone

HRID 1433156
노트
인쇄 미리보기

반응식

HRID 1433156 반응식
[CH2:1]([O:8][C:9]([N:11]1[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:17]([O:24][C:25]1[CH:26]=[C:27]([NH:35][C:36](=[O:38])[CH3:37])[CH:28]=[CH:29][C:30]=1[C:31](=[O:34])[CH2:32]Br)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[C:36]([NH:35][C:27]1[CH:28]=[CH:29][C:30]([C:31](=[O:34])[CH2:32][N:14]2[CH2:15][CH2:16][N:11]([C:9]([O:8][CH2:1][C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=3)=[O:10])[CH2:12][CH2:13]2)=[C:25]([O:24][CH2:17][C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=2)[CH:26]=1)(=[O:38])[CH3:37]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 643495Benzyl piperazine-1-carboxylateHCID 85606679N-[3-benzyloxy-4-(2-bromo-acetyl)phenyl]-acetamide

생성물 1

HCID 690575444'-Acetamido-2'-benzyloxy-2-[4-(benzyloxycarbonyl)piperazin-1-yl]acetophenone수율 41.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

1-(Benzyloxycarbonyl)piperazine (117 μL, 134 mg, 0.607 mmol) was added to a mixture of N-[3-benzyloxy-4-(2-bromo-acetyl)phenyl]-acetamide (200 mg, 0.552 mmol) and potassium carbonate (115 mg, 0.828 mmol) in DMF (5 mL), and stirred at room temperature for 18 hours. The solvent was removed in vacuo, and taken up in brine (25 mL). The aqueous was extracted with DCM (3×25 mL) and the combined organics dried (MgSO4). The solvents were removed in vacuo, and the product was purified by preparative HPLC to give pure 4′-acetamido-2′-benzyloxy-2-[4-(benzyloxycarbonyl)piperazin-1-yl]acetophenone (114 mg, 41%, 50% rec.) as an off-white solid; δH (CDCl3) 8.23 (1H, br s), 7.81 (1H, d, J=8.6 Hz), 7.77-7.76 (1H, m), 7.53-7.51 (2H, m), 7.42-7.28 (8H, m), 7.08 (1H, dd, J=8.6, 1.8 Hz), 5.20 (2H, s), 5.12 (2H, s), 4.00 (2H, s), 3.59-3.48 (4H, m), 2.65-2.60 (4H, m), 2.14 (3H, s); LCMS retention time 2.07 min, M+H+ 502.5, along with recovered N-(4-acetyl-3-benzyloxy-phenyl)-acetamide (35 mg).

후처리

  1. customThe solvent was removed in vacuo
  2. extractionThe aqueous was extracted with DCM (3×25 mL)
  3. dry with materialthe combined organics dried (MgSO4)
  4. customThe solvents were removed in vacuo
  5. customthe product was purified by preparative HPLC

출처 및 근거

ORD 기록
ord-563f8ad0daf74a0eb68aadd7d6a69792
출처 데이터셋
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07612201B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트