Water → 2-(7-Methyl-2,3-dihydro-1,4-benzodioxin-2-yl)ethan-1-ol

HRID 2419102ノート

反応式

HRID 2419102 の反応式
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]2[O:10][CH2:9][CH:8]([CH2:11][C:12](O)=[O:13])[O:7][C:6]=2[CH:15]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1>[OH:13][CH2:12][CH2:11][CH:8]1[O:7][C:6]2[CH:15]=[C:2]([CH3:1])[CH:3]=[CH:4][C:5]=2[O:10][CH2:9]1

参加物

6

反応物 4

HCID 962Water2 回HCID 14798Sodium HydroxideHCID 20540154(7-Methyl-2,3-dihydro-1,4-benzodioxin-2-yl)acetic acidHCID 21226445Aluminium lithium hydride

生成物 1

HCID 128506052-(7-Methyl-2,3-dihydro-1,4-benzodioxin-2-yl)ethan-1-ol

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

The preparation of various new starting materials is illustrated as follows: The solution of 48.6 g of 2-(7-methyl-1,4-benzodioxan-2-yl)-acetic acid in the minimum amount of tetrahydrofuran is added dropwise at reflux rate to the stirred suspension of 13.4 g of lithium aluminum hydride in 200 ml dry tetrahydrofuran. The mixture is refluxed overnight, cooled, and decomposed by the addition of 13.4 ml of water, 13.4 ml 15% aqueous sodium hydroxide and 40 ml of water. It is filtered, evaporated, the residue distilled in a molecular still, and the fraction boiling at 155°-165°/0.1 mm Hg collected as colorless oil, to yield the 2-(2-hydroxyethyl)-7-methyl-1,4-benzodioxan.

後処理

  1. customThe preparation of various new starting materials
  2. temperatureat reflux rate
  3. temperatureThe mixture is refluxed overnight
  4. temperaturecooled
  5. filtrationIt is filtered
  6. customevaporated
  7. distillationthe residue distilled in a molecular still, and the fraction boiling at 155°-165°/0.1 mm Hg
  8. customcollected as colorless oil

出典と根拠

ORDレコード
ord-aac6784379c14a299bb90845a7a9e9ff
出典データセット
uspto-grants-1978_08
特許番号
US04104396

反応ノート

読み込み中…