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

HRID 2209651

반응식

HRID 2209651 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 140282113,4-Dihydroxy-5-iodobenzaldehyde수율 66.2%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
0 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-0758a9a2538c48aba71aa6ea82c5a870
출처 데이터셋
uspto-grants-1995_10
특허 번호
US05455238

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