Water → 6-benzyloxy-2H-1-benzopyran-3-carboxaldehyde

HRID 466175

反応式

HRID 466175 の反応式
[OH:1][C:2]1[CH:3]=[CH:4][C:5]2[O:10][CH2:9][C:8]([CH:11]=[O:12])=[CH:7][C:6]=2[CH:13]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:20](Br)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.O>CN(C=O)C>[CH2:20]([O:1][C:2]1[CH:3]=[CH:4][C:5]2[O:10][CH2:9][C:8]([CH:11]=[O:12])=[CH:7][C:6]=2[CH:13]=1)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1

参加物

6

反応物 4

HCID 962WaterHCID 7498Benzyl BromideHCID 11430Potassium CarbonateHCID 47708156-Hydroxychromene-3-carboxaldehyde

生成物 1

HCID 149712606-benzyloxy-2H-1-benzopyran-3-carboxaldehyde

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 6-hydroxy-2H-1-benzopyran-3-carboxaldehyde (25.0 g, 0.14 mol) and potassium carbonate (39.2 g, 0.28 mol) in 500 ml of DMF is treated with benzyl bromide (26.7 g, 0.16 mol). The mixture is stirred overnight at room temperature. Water is added and three extractions with dichloromethane are carried out. The extract is dried (MgSO4) and evaporated to dryness. The residue is crystallized from hot ethyl acetate to give 6-benzyloxy-2H-1-benzopyran-3-carboxaldehyde, m.p. 112°-114° C.

後処理

  1. extractionthree extractions with dichloromethane
  2. dry with materialThe extract is dried (MgSO4)
  3. customevaporated to dryness
  4. customThe residue is crystallized from hot ethyl acetate

出典と根拠

ORDレコード
ord-12f6cde40e39456691a1140d3910462e
出典データセット
uspto-grants-1992_10
特許番号
US05155130

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