N,N-Dimethylaniline → HCID 69250913, 화합물

HRID 2223994노트

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HRID 2223994 반응식
[OH:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][O:8][C:9]1[CH:17]=[CH:16][C:12]([C:13]([OH:15])=[O:14])=[C:11]([F:18])[CH:10]=1.CN(C)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.[O:28]1C[CH2:31][CH2:30][CH2:29]1.C(Cl)(=O)C=C>C(C1C(O)=C(CCCC)C=C(C)C=1)CCC.O>[C:29]([CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:21][O:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][O:8][C:9]1[CH:17]=[CH:16][C:12]([C:13]([OH:15])=[O:14])=[C:11]([F:18])[CH:10]=1)(=[O:28])[CH:30]=[CH2:31]

참가 물질

7

반응물 4

HCID 949N,N-DimethylanilineHCID 8028TetrahydrofuranHCID 13140Acryloyl chlorideHCID 69251770HCID 69251770, 화합물

생성물 1

HCID 69250913HCID 69250913, 화합물

시약·촉매·용매 2

HCID 111175752,6-Dibutyl-4-methylphenol촉매HCID 962Water용매

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온도
60 °C

실험 절차

Under a nitrogen atmosphere, 4-(6-hydroxyhexyloxy)-2-fluorobenzoic acid (189 g), N,N-dimethylaniline (133 g) and 2,6-dibutyl-p-cresol (0.80 g) were added to tetrahydrofuran (500 mL). Acrylic acid chloride (100 g) was added dropwise thereto, followed by agitating at 60° C. for 3 hours. The reaction solution was poured into water and extracted with ethyl acetate. The organic layer was washed with hydrochloric acid, a saturated sodium hydrogencarbonate aqueous solution and water, and after drying over anhydrous magnesium sulfate, the solvent was distilled off under reduced pressure. The resulting residue was recrystallized from ethanol to obtain 4-(6-acryloylhexyloxyhexyloxy)-2-fluorobenzoic acid (141 g).

후처리

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with hydrochloric acid
  3. dry with materiala saturated sodium hydrogencarbonate aqueous solution and water, and after drying over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. customThe resulting residue was recrystallized from ethanol

출처 및 근거

ORD 기록
ord-ca72d716246f4bfab9b90c9e30af08c1
출처 데이터셋
uspto-grants-2008_05
특허 번호
US07378135B2

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