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Potassium Carbonate → HCID 68922176、化合物

HRID 1804687
ノート
印刷プレビュー

反応式

HRID 1804687 の反応式
Cl[CH2:2][O:3][C:4](=[O:15])[CH:5]([NH:7][C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])[CH3:6].[CH2:16]([N:18]1[C:23]([C:24]([C:26]2[CH:27]=[C:28]([CH:31]=[C:32]([CH3:34])[CH:33]=2)[C:29]#[N:30])=[O:25])=[C:22]([CH:35]([CH3:37])[CH3:36])[C:21](=[O:38])[NH:20][C:19]1=[O:39])[CH3:17].C([O-])([O-])=O.[K+].[K+]>CN(C=O)C.[I-].C([N+](CCCC)(CCCC)CCCC)CCC>[C:29]([C:28]1[CH:27]=[C:26]([CH:33]=[C:32]([CH3:34])[CH:31]=1)[C:24]([C:23]1[N:18]([CH2:16][CH3:17])[C:19](=[O:39])[N:20]([CH2:2][O:3][C:4](=[O:15])[CH:5]([NH:7][C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])[CH3:6])[C:21](=[O:38])[C:22]=1[CH:35]([CH3:37])[CH3:36])=[O:25])#[N:30]
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 3

HCID 11430Potassium CarbonateHCID 25215428AinuovirineHCID 72978647HCID 72978647、化合物

生成物 1

HCID 68922176HCID 68922176、化合物収率 71.4%

試薬・触媒・溶媒 2

HCID 67553Tetrabutylammonium Iodide触媒HCID 6228Dimethylformamide
溶媒

実験手順

To a solution of 2-tert-butoxycarbonylamino-propionic acid chloromethyl ester (4) (0.6207 g, 2.61 mmol) and 3-(3-ethyl-5-isopropyl-2,6-dioxo-1,2,3,6-tetrahydro-pyrimidine-4-carbonyl)-5-methyl-benzonitrile (0.780 g, 2.40 mmol) in DMF (10 mL) was added K2CO3 and tetrabutylammonium iodide (0.193 g, 0.522 mmol), and the reaction mixture stirred for 48 h. The reaction mixture was concentrated, diluted with ethyl acetate and washed with H2O (2×), brine, dried (MgSO4) and concentrated. The residue was purified by flash column chromatography (silica gel, 0 to 50% ethyl acetate/hexane) to give a yellow foam (5) (0.9028 g, 71%). 1H NMR (300 MHz, CDCl3): 8.01 (s, 1H), 7.94 (s, 1H), 7.77 (s, 1H), 6.1-5.9 (m, 2H), 5.05 (br s, 1H), 4.32 (br s, 1H), 3.9-3.8 (m, 1H), 3.2-3.1 (m, 1H), 2.49 (s, 3H), 2.2-2.1 (m, 1H), 1.39 (s, 9H), 1.37 (s, 3H), 1.2-1.1 (m, 9H). Mass spectrum: 549.1 (M+Na).

後処理

  1. concentrationThe reaction mixture was concentrated
  2. additiondiluted with ethyl acetate
  3. washwashed with H2O (2×), brine
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated
  6. customThe residue was purified by flash column chromatography (silica gel, 0 to 50% ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-ce583a7fbb2e4b34aa9a791b23c7c778
出典データセット
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08354421B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート