Hydrochloric Acid → HCID 20161182、化合物

HRID 247018ノート

反応式

HRID 247018 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][C:11]=1[O:12][CH3:13])[CH2:8][C:7]([C:14]#N)=[CH:6]2.[H-].C([Al+]CC(C)C)C(C)C.C[OH:27].Cl>C1(C)C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][C:11]=1[O:12][CH3:13])[CH2:8][C:7]([CH:14]=[O:27])=[CH:6]2

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 20161200HCID 20161200、化合物HCID 21225700Diisobutylaluminumhydride

生成物 1

HCID 20161182HCID 20161182、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

反応条件

温度
-5 °C

実験手順

5,6-Dimethoxy-1H-indene-2-carbonitrile (1.8 g) was suspended in dry toluene (40 ml) under an atmosphere of nitrogen. The reaction mixture was cooled to -5° C. and treated dropwise with a solution of diisobutylaluminium hydride in toluene (1.5M, 13 ml). After 30 minutes the solution was treated with methanol (5 ml) then poured into hydrochloric acid (1M, 200 ml) and stirred for 15 minutes. The resultant solution was extracted into dichloromethane (4×100 ml) then the organic extracts were combined, washed with brine, dried over magnesium sulphate and evaporated to dryness. The residue (1.4 g) was crystallised from dichloromethane:ether to give 5,6-dimethoxy-1-H-indene-2-carboxaldehyde as a white solid, m.p. 125°-128° C.

後処理

  1. extractionThe resultant solution was extracted into dichloromethane (4×100 ml)
  2. washwashed with brine
  3. dry with materialdried over magnesium sulphate
  4. customevaporated to dryness
  5. customThe residue (1.4 g) was crystallised from dichloromethane

出典と根拠

ORDレコード
ord-09f438ec31564fc782eae76b2e281f46
出典データセット
uspto-grants-1987_11
特許番号
US04705782

反応ノート

読み込み中…