Water → HCID 58820701, 화합물

HRID 458481

반응식

HRID 458481 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

HCID 58820701HCID 58820701, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
50 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-07b28ce665fb4c639f8a601b30a280bc
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07192650B2

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