HCID 20284765、化合物 → 4-Formyl-2,3,4,9-tetrahydrothiopyrano[2,3-b]indole

HRID 127514

反応式

HRID 127514 の反応式
[OH:1][CH2:2][C:3]#[C:4][CH2:5][S:6][C:7]1[NH:8][C:9]2[C:14]([CH:15]=1)=[CH:13][CH:12]=[CH:11][CH:10]=2>N1C=CC=CC=1>[CH:2]([CH:3]1[C:15]2[C:14]3[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=3)[NH:8][C:7]=2[S:6][CH2:5][CH2:4]1)=[O:1]

参加物

3

反応物 1

HCID 20284765HCID 20284765、化合物

生成物 1

HCID 147356294-Formyl-2,3,4,9-tetrahydrothiopyrano[2,3-b]indole収率 67.8%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A solution of the product of the above (1) (12.0 g) in pyridine (120 ml) is heated at 100° C. for 2 hours and evaporated to remove the pyridine. The residue is dissolved in ether (300 ml), washed with water, 2 N hydrochloric acid and a saturated saline solution, dried and evaporated to remove the solvent. The residue (11.0 g) is chromatographed on silica gel (50 g) and eluted with benzene. The eluate is evaporated to give the title compound as an oil (8.14 g). The oil is gradually solidified in a refrigerator.

後処理

  1. customevaporated
  2. customto remove the pyridine
  3. dissolutionThe residue is dissolved in ether (300 ml)
  4. washwashed with water, 2 N hydrochloric acid
  5. customa saturated saline solution, dried
  6. customevaporated
  7. customto remove the solvent
  8. customThe residue (11.0 g) is chromatographed on silica gel (50 g)
  9. washeluted with benzene
  10. customThe eluate is evaporated

出典と根拠

ORDレコード
ord-92bc557fabfd4287adee9bad8db427cd
出典データセット
uspto-grants-1981_03
特許番号
US04256640

関連ノート

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