Boron tribromide → 3,4-Dihydroxy-5-iodobenzaldehyde

HRID 727406

反応式

HRID 727406 の反応式
[I:1][C:2]1[C:3]([OH:12])=[C:4]([O:10]C)[CH:5]=[C:6]([CH:9]=1)[CH:7]=[O:8].B(Br)(Br)Br>ClCCl>[I:1][C:2]1[CH:9]=[C:6]([CH:5]=[C:4]([OH:10])[C:3]=1[OH:12])[CH:7]=[O:8]

参加物

4

反応物 2

HCID 25134Boron tribromideHCID 79499Benzaldehyde, 4-hydroxy-3-iodo-5-methoxy-

生成物 1

HCID 140282113,4-Dihydroxy-5-iodobenzaldehyde収率 66.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

37.2 g of 5-iodo vanillin (commercial) and 360 ml of dichloromethane were mixed together under nitrogen and the mixture was cooled to 0° C. 135 ml of a molar solution of boron tribromide in dichloromethane were added and the mixture stood for 16 hours at ambient temperature and was then concentrated, cooled to 0° C. and acidified. The crystallized product was separated out, washed with water, dried and crystallized from an isopropanol-water mixture (1-2 by volume) to obtain 23.4 g of the expected product.

後処理

  1. concentrationwas then concentrated
  2. temperaturecooled to 0° C.
  3. customThe crystallized product was separated out
  4. washwashed with water
  5. customdried
  6. customcrystallized from an isopropanol-water mixture (1-2 by volume)

出典と根拠

ORDレコード
ord-a599db6ba9bd4155b386f14fe3904811
出典データセット
uspto-grants-1998_01
特許番号
US05712266

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