Water → HCID 58820701、化合物

HRID 458481

反応式

HRID 458481 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8]([OH:10])[CH:9]=1)[CH:5]=[O:6].[C:11]([O-:14])([O-])=O.[K+].[K+].Br[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][OH:28].O>CN(C=O)C>[OH:28][CH2:27][CH2:26][CH2:25][CH2:24][CH2:23][CH2:22][CH2:21][CH2:20][CH2:19][CH2:18][O:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8]([O:10][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:11][OH:14])[CH:9]=1)[CH:5]=[O:6]

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 943653,5-DihydroxybenzaldehydeHCID 1045071-Decanol, 10-bromo-

生成物 1

HCID 58820701HCID 58820701、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
50 °C

実験手順

1.18 g of 3,5-dihydroxybenzaldehyde A-2 (8.56 mmol) and 6.15 g of K2CO3 (44.5 mmol, 5.2 eq.) were added to 4.47 g of 10-bromodecane-1-ol A-1 (18.8 mmol, 2.2 eq.) dissolved in 100 mL of DMF, and the mixture was stirred in nitrogen atmosphere at 50° C. for 48 hours. After the temperature was returned to room temperature, the reaction was stopped by adding 50 mL of water and the organic layer was extracted with ether (100 mL×3). The extracted organic layers were combined, washed with saturated brine and dried with anhydrous Na2SO4. The solvent was removed by using an evaporator, whereby brown liquid A-3 was obtained (crude yield: 4.418 g). The product was not purified at this stage and directly used for the next reaction.

後処理

  1. customwas returned to room temperature
  2. extractionthe organic layer was extracted with ether (100 mL×3)
  3. washwashed with saturated brine
  4. dry with materialdried with anhydrous Na2SO4
  5. customThe solvent was removed
  6. customan evaporator, whereby brown liquid A-3
  7. customwas obtained (crude yield: 4.418 g)
  8. customThe product was not purified at this stage
  9. customdirectly used for the next reaction

出典と根拠

ORDレコード
ord-07b28ce665fb4c639f8a601b30a280bc
出典データセット
uspto-grants-2007_03
特許番号
US07192650B2

関連ノート

読み込み中…