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

HRID 466175

반응식

HRID 466175 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-12f6cde40e39456691a1140d3910462e
출처 데이터셋
uspto-grants-1992_10
특허 번호
US05155130

연결된 노트

불러오는 중…