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Water → HCID 25215195, 화합물

HRID 2194770
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HRID 2194770 반응식
[C:1]([C:3]1[CH:4]=[C:5]([CH:36]=[C:37]([CH3:39])[CH:38]=1)[C:6]([C:8]1[N:13]([CH2:14][C:15]2([CH2:18][C:19]([NH:21]CC3C=CC(OC)=CC=3)=[O:20])[CH2:17][CH2:16]2)[C:12](=[O:31])[NH:11][C:10](=[O:32])[C:9]=1[CH:33]([CH3:35])[CH3:34])=[O:7])#[N:2].O>C(#N)C.C(O)(=O)C.C(OCC)(=O)C>[C:1]([C:3]1[CH:4]=[C:5]([CH:36]=[C:37]([CH3:39])[CH:38]=1)[C:6]([C:8]1[N:13]([CH2:14][C:15]2([CH2:18][C:19]([NH2:21])=[O:20])[CH2:16][CH2:17]2)[C:12](=[O:31])[NH:11][C:10](=[O:32])[C:9]=1[CH:33]([CH3:35])[CH3:34])=[O:7])#[N:2]
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참가 물질

6

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HCID 962WaterHCID 582034682-{1-[6-(3-cyano-5-methyl-benzoyl)-5-isopropyl-2,4-dioxo-3,4-dihydro-2H-pyrimidin-1-ylmethyl]-cyclopropyl}-N-(4-methoxy-benzyl)-acetamide

생성물 1

HCID 25215195HCID 25215195, 화합물수율 80.2%

시약·촉매·용매 3

HCID 176Acetic Acid용매HCID 6342Acetonitrile용매
HCID 8857
Ethyl Acetate
용매

실험 절차

To a stirred solution of 2-{1-[6-(3-cyano-5-methyl-benzoyl)-5-isopropyl-2,4-dioxo-3,4-dihydro-2H-pyrimidin-1-ylmethyl]-cyclopropyl}-N-(4-methoxy-benzyl)-acetamide (97 mg, 0.18 mmol) in acetonitrile (4 mL) and glacial acetic acid (1 mL) at room temperature, were added ceric ammonium nitrate (201 mg, 0.36 mmol) and water (2 mL) in this order. After stirring for 20 min., the mixture was diluted with ethyl acetate, washed with water twice, dried with MgSO4, filtered, and evaporated in vacuo. The residue was purified by silica gel column chromatography (eluent, from ethyl acetate to 10% methanol in ethyl acetate) to give 59 mg (78%) of 2-{1-[6-(3-cyano-5-methyl-benzoyl)-5-isopropyl-2,4-dioxo-3,4-dihydro-2H-pyrimidin-1-ylmethyl]-cyclopropyl}-acetamide (85) as a white solid. m.p. 283-285° C.; 1H-NMR (500 MHz, DMSO-d6) δ 0.20-0.27 (2H, m), 0.31-0.36 (1H, m), 0.43-0.47 (1H, m), 0.99 (3H, d, J=6.8 Hz), 1.08 (3H, d, J=6.8 Hz), 2.02-2.13 (2H, m), 2.17 (1H, d, J=16.5 Hz), 2.44 (3H, s), 3.32 (1H, d, J=15.1 Hz), 3.39-3.41 (1H, m), 3.46-3.51 (1H, m), 3.79 (1H, d, J=15.1 Hz), 8.08 (1H, s), 8.19 (1H, s), 8.42 (1H, s), 11.45 (1H, s); m/z (EI) 408 (M+).

후처리

  1. washwashed with water twice
  2. dry with materialdried with MgSO4
  3. filtrationfiltered
  4. customevaporated in vacuo
  5. customThe residue was purified by silica gel column chromatography (eluent, from ethyl acetate to 10% methanol in ethyl acetate)

출처 및 근거

ORD 기록
ord-990a7daf1a5c45d08482953b79a9e795
출처 데이터셋
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08334295B2

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