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Sodium Iodide → 4-Methylpentyl 5-(tetradecyloxy)furan-2-carboxylate

HRID 57219
ノート
印刷プレビュー

反応式

HRID 57219 の反応式
[CH2:1]([O:15][C:16]1[O:20][C:19]([C:21]([OH:23])=[O:22])=[CH:18][CH:17]=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][CH3:14].Br[CH2:25][CH2:26][CH2:27][CH:28]([CH3:30])[CH3:29].C(=O)([O-])[O-].[Cs+].[Cs+].[I-].[Na+]>CN(C)C=O.CCOC(C)=O.[Cl-].[Na+].O.O>[CH2:1]([O:15][C:16]1[O:20][C:19]([C:21]([O:23][CH2:25][CH2:26][CH2:27][CH:28]([CH3:30])[CH3:29])=[O:22])=[CH:18][CH:17]=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][CH3:14]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 4

HCID 5238Sodium IodideHCID 10796Cesium carbonateHCID 69385Pentane, 1-bromo-4-methyl-HCID 1151755-(Tetradecyloxy)-2-furoic acid2 回

生成物 1

HCID 668698124-Methylpentyl 5-(tetradecyloxy)furan-2-carboxylate収率 62.2%

試薬・触媒・溶媒 4

HCID 962
Water
溶媒
HCID 6228Dimethylformamide溶媒
HCID 8857Ethyl Acetate溶媒
HCID 57417360Sodium chloride; water溶媒

実験手順

To a vigorously stirred suspension of 5-(tetradecyloxy)furan-2-carboxylic acid (0.162 g, 0.5 mmol) in 10 mL of N,N-dimethylformamide was added 1-bromo-4-methylpentane (0.247 g, 1.5 mmol), cesium carbonate (0.243 g, 0.75 mmol) and sodium iodide (˜20 mg). The suspension appeared to go into solution briefly, and then a very finely dispersed white precipitate was observed. The reaction was allowed to stir for 12 hrs at which time HPLC analysis of the reaction solution indicated complete conversion of TOFA to a less polar product. The suspension was diluted with EtOAc (40 mL), brine (20 mL) and water (20 mL). The phases were separated and the organic phase was washed with water (20 mL) and brine (20 mL) and then dried and concentrated. The resulting crude material was purified by flash chromatography eluting with 0-20% EtOAc in hexanes to yield 0.127 g (62%) of the title compound. 1H NMR (300 MHz, CDCl3) δ: 7.15 (d, 1H), 5.30 (d, 1H), 4.22 (t, 2H), 4.10 (t, 2H), 1.18-1.80 (m, 29H), 0.89 (t, 9H).

後処理

  1. customThe phases were separated
  2. washthe organic phase was washed with water (20 mL) and brine (20 mL)
  3. customdried
  4. concentrationconcentrated
  5. customThe resulting crude material was purified by flash chromatography
  6. washeluting with 0-20% EtOAc in hexanes

出典と根拠

ORDレコード
ord-06c8b30c5e0f4d0090984b9d5fe78529
出典データセット
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09434718B2

反応ノート

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