Phenethyl isocyanate → HCID 67904965、化合物

HRID 465638ノート

反応式

HRID 465638 の反応式
[CH2:1]([NH:19][CH2:20][C:21]([NH:23][C:24]1[C:29]([O:30][CH3:31])=[CH:28][C:27]([O:32][CH3:33])=[CH:26][C:25]=1[O:34][CH3:35])=[O:22])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8]/[CH:9]=[CH:10]\[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18].[CH:36]1[CH:41]=[CH:40][C:39]([CH2:42][CH2:43][N:44]=[C:45]=[O:46])=[CH:38][CH:37]=1>C(OCC)(=O)C>[CH2:1]([N:19]([C:45]([NH:44][CH2:43][CH2:42][C:39]1[CH:40]=[CH:41][CH:36]=[CH:37][CH:38]=1)=[O:46])[CH2:20][C:21]([NH:23][C:24]1[C:29]([O:30][CH3:31])=[CH:28][C:27]([O:32][CH3:33])=[CH:26][C:25]=1[O:34][CH3:35])=[O:22])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8]/[CH:9]=[CH:10]\[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18]

参加物

4

反応物 2

HCID 160602Phenethyl isocyanateHCID 67904675HCID 67904675、化合物

生成物 1

HCID 67904965HCID 67904965、化合物

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 0.50 g of the product of Example 7, 0.2 g 2-phenethyl isocyanate, and a few mL ethyl acetate were briefly heated on the steambath and then allowed to sit 3 days at room temperature. The reaction mixture was then washed with dilute H3PO4, NaHCO3, and HaCl solutions, dried over MgSO4, filtered, and concentrated to an oil. The oil was chromatographed on SiO2 (70-230 mesh) using EtoAc as eluant. The product was obtained as an oil which crystallized on standing. 0.28 g (44%). NMR (CDCl3) δ 0.88 (3H, t), δ 1.25 (24H, m), δ 1.96 (4H, m) δ 2.84 (2H, t), δ 3.23 (2H, t), δ 3.51 (2H, q), δ 3.69 (6H, s), δ 3.77 (3H, s), δ 4.03 (2H, s), δ 4.70 (1H, t), δ 5.35 (2H, t), δ 6.13 (2H, s), δ 7.16-7.31 (5H, m), δ 7.46 (1H, s). IR (KBr) 3251, 2925, 1662, 1621, 1533, 1465, 1156, 1128, 810 cm-1.

後処理

  1. washThe reaction mixture was then washed with dilute H3PO4, NaHCO3, and HaCl solutions
  2. dry with materialdried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated to an oil
  5. customThe oil was chromatographed on SiO2 (70-230 mesh)
  6. customThe product was obtained as an oil which
  7. customcrystallized

出典と根拠

ORDレコード
ord-429fe8f295234d2d948b2d89cdcffdcd
出典データセット
uspto-grants-1992_10
特許番号
US05153226

反応ノート

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