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Hydrochloric Acid → HCID 58788081、化合物

HRID 1917587
ノート
印刷プレビュー

反応式

HRID 1917587 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([CH:9]=[C:10]([OH:12])[CH:11]=1)[C:5]([O:7][CH3:8])=[O:6].C([O-])([O-])=O.[K+].[K+].Br[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH3:31].Cl>CN(C=O)C>[CH2:20]([O:1][C:2]1[CH:3]=[C:4]([CH:9]=[C:10]([O:12][CH2:31][CH2:30][CH2:29][CH2:28][CH2:27][CH2:26][CH2:25][CH2:24][CH2:23][CH2:22][CH2:21][CH3:20])[CH:11]=1)[C:5]([O:7][CH3:8])=[O:6])[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH3:31]
参加物反応条件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 313Hydrochloric AcidHCID 89191-BromododecaneHCID 11430Potassium CarbonateHCID 75076Methyl 3,5-Dihydroxybenzoate

生成物 1

HCID 58788081HCID 58788081、化合物収率 75%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

Methyl 3,5-dihydroxybenzoate (4.2 g, 25 mmol) was dissolved in 25 mL of dry DMF and then 13.86 g (100 mmol) of K2CO3 was added in the reaction mixture, where the above mixture was stirred at 80° C. for 1 h under a N2 atmosphere and then 1-bromododecane (12.4 g, 50 mmol) was added dropwise to the reaction mixture. The reaction mixture was stirred at 90° C. for 24 h under N2. At the end of the reaction, the mixture was poured onto ice, 2N—HCl and extracted with MC, H20, NaHCO3 and brine. The solvent was removed in vacuo. The crude solid was purified by column chromatograph with 10% EA and hexane to yield 75% of the product. 1H-NMR (300 MHz, CDCl3) δ 7.1 (d, 2H), 6.6 (t, 1H), 4.0 (t, 4H), 3.9 (s, OCH3), 1.7-1.8 (m, 4H), 1.4-1.6 (m, 4H), 1.1-1.3 (m, 32H), 0.9 (t, 6H).

後処理

  1. stirringThe reaction mixture was stirred at 90° C. for 24 h under N2
  2. customAt the end of the reaction
  3. extractionextracted with MC, H20, NaHCO3 and brine
  4. customThe solvent was removed in vacuo
  5. customThe crude solid was purified by column chromatograph with 10% EA and hexane

出典と根拠

ORDレコード
ord-1503100fd0a140e4b6c166bd9dff28a2
出典データセット
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08618298B2

反応ノート

読み込み中…

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