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Triethylamine → HCID 67323709、化合物

HRID 896726
ノート
印刷プレビュー

反応式

HRID 896726 の反応式
[CH2:1]([O:17][C:18](=[O:35])[CH:19]=[CH:20][C:21]1[CH:26]=[CH:25][C:24]([O:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][OH:34])=[CH:23][CH:22]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16].C(N(CC)CC)C.[C:43](Cl)(=[O:47])[C:44]([CH3:46])=[CH2:45].[OH-].[K+]>O1CCCC1>[CH2:1]([O:17][C:18]([CH:19]=[CH:20][C:21]1[CH:26]=[CH:25][C:24]([O:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][O:34][C:43](=[O:47])[C:44]([CH3:46])=[CH2:45])=[CH:23][CH:22]=1)=[O:35])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16]
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 4

HCID 8471TriethylamineHCID 13528Methacryloyl chlorideHCID 14797Potassium HydroxideHCID 69764959HCID 69764959、化合物

生成物 1

HCID 67323709HCID 67323709、化合物収率 12.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To an ice-cooled solution of 3-[4-(6-hydroxy-hexyloxy)-phenyl]-acrylic acid hexadecyl ester (2.6 g, 5.3 mmol), triethylamine (0.99 ml, 7.4 mmol) and 4 crystals of BHT in tetrahydrofuran (30 ml) was added dropwise methacryloyl chloride (0.68 g, 6.9 mmol). The reaction mixture was allowed to react for 7.5 hours, warming to room temperature. Potassium hydroxide solution (5 wt %, 50 ml) was added and the solution extracted 3×100 ml ethyl acetate. The combined organic layers were washed with 100 ml portions of 1M HCl, water, brine and then dried with magnesium sulfate and concentrated. The crude product was purified by silica gel chromatography eluting with 10% ethyl acetate in hexane, followed by recrystallization from hexane, to give 0.37 g white solid, 95% pure by HPLC. H1 NMR (CDCl3): 7.65 (d, 1H, J=16 Hz), 7.49 (d, 2H, J=8.7 Hz), 6.90 (d, 2H, J=8.8 Hz), 6.33 (d, 1H, J=15.8 Hz), 6.12 (m, 1H), 5.57 (m, 1H), 4.19 (m, 4H), 4.00 (m, 2H), 1.96 (m, 3H), 1.8-1.4 (m, 8H), 1.28 (s, 32H), 0.90 (vt, 3H).

後処理

  1. customto react for 7.5 hours
  2. extractionthe solution extracted 3×100 ml ethyl acetate
  3. washThe combined organic layers were washed with 100 ml portions of 1M HCl, water, brine
  4. dry with materialdried with magnesium sulfate
  5. concentrationconcentrated
  6. customThe crude product was purified by silica gel chromatography
  7. washeluting with 10% ethyl acetate in hexane
  8. customfollowed by recrystallization from hexane

出典と根拠

ORDレコード
ord-957a3731669f4af288f545e05eb16e9d
出典データセット
uspto-grants-2005_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06919404B2

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