Water → HCID 22123617, 화합물

HRID 1859334노트

반응식

HRID 1859334 반응식
O[C:2]1([C:26]2[CH:31]=[CH:30][C:29]([O:32][CH2:33][CH2:34][N:35]3[CH2:40][CH2:39][CH2:38][CH2:37][CH2:36]3)=[CH:28][CH:27]=2)[C:7]2[CH:8]=[CH:9][C:10]([O:12]COC)=[CH:11][C:6]=2[O:5][CH2:4][CH:3]1[C:16]1[CH:21]=[CH:20][C:19]([O:22]COC)=[CH:18][CH:17]=1.[NH+]1C=CC=CC=1.O>CO>[OH:12][C:10]1[CH:9]=[CH:8][C:7]2[C:2]([C:26]3[CH:31]=[CH:30][C:29]([O:32][CH2:33][CH2:34][N:35]4[CH2:36][CH2:37][CH2:38][CH2:39][CH2:40]4)=[CH:28][CH:27]=3)=[C:3]([C:16]3[CH:21]=[CH:20][C:19]([OH:22])=[CH:18][CH:17]=3)[CH2:4][O:5][C:6]=2[CH:11]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 4989215PyridiniumHCID 22123586HCID 22123586, 화합물

생성물 1

HCID 22123617HCID 22123617, 화합물수율 37%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

4-Hydroxy-7-methoxymethyloxy-3-[4-(methoxymethyloxy)phenyl]-4-[4-(piperidinoethyloxy)phenyl]-2,3-dihydro-4H-benzopyran (83 mg, 0.14 mmol) and pyridinium p-toulenesulfonate (214 mg, 1.4 mmol) were dissolved in methanol (6 ml) and then refluxed for 12 hours. The reaction solution was cooled to room temperature and, after adding water, extracted with ethyl acetate. The organic layer thus separated was dried over anhydrous magnesium sulfate, filtered and then concentrated under reduced pressure to remove the organic solvent. The residue was separated by column chromatography (n-hexane:ethyl acetate=1:4) to obtain 23 mg (yield: 37%) of the title compound as a foam.

후처리

  1. temperaturerefluxed for 12 hours
  2. extractionextracted with ethyl acetate
  3. customThe organic layer thus separated
  4. dry with materialwas dried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customto remove the organic solvent
  8. customThe residue was separated by column chromatography (n-hexane:ethyl acetate=1:4)

출처 및 근거

ORD 기록
ord-3968e6eb9b424b6fb4e51327917542f5
출처 데이터셋
uspto-grants-2000_11
특허 번호
US06153768

반응 노트

불러오는 중…