Water → HCID 22123617、化合物

HRID 1859334ノート

反応式

HRID 1859334 の反応式
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

参加物

5

反応物 3

HCID 962WaterHCID 4989215PyridiniumHCID 22123586HCID 22123586、化合物

生成物 1

HCID 22123617HCID 22123617、化合物収率 37%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-3968e6eb9b424b6fb4e51327917542f5
出典データセット
uspto-grants-2000_11
特許番号
US06153768

反応ノート

読み込み中…