Boron tribromide → 5-Formyl-2,3-dihydroxybenzonitrile

HRID 428825

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HRID 428825 반응식
[CH:1]([C:3]1[CH:4]=[C:5]([C:8]([OH:13])=[C:9]([O:11]C)[CH:10]=1)[C:6]#[N:7])=[O:2].B(Br)(Br)Br>ClCCl>[CH:1]([C:3]1[CH:4]=[C:5]([C:8]([OH:13])=[C:9]([OH:11])[CH:10]=1)[C:6]#[N:7])=[O:2]

참가 물질

4

반응물 2

HCID 25134Boron tribromideHCID 18359065Benzonitrile, 5-formyl-2-hydroxy-3-methoxy-

생성물 1

HCID 152925835-Formyl-2,3-dihydroxybenzonitrile수율 72.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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온도
0 °C

실험 절차

18 g of the product of Step A and 400 ml of dichloromethane were mixed together under nitrogen and the mixture was cooled to 0° C. 150 ml of a molar solution of boron tribromide in dichloromethane were added and the mixture stood for one night at ambient temperature. It was concentrated, cooled again to 0° C. and 250 ml of a normal solution of hydrochloric acid were added. The crystallized product was separated out, washed with water, dried then crystallized from an isopropanol—water mixture (1-2) to obtain 12 g of the expected product.

후처리

  1. waitthe mixture stood for one night at ambient temperature
  2. concentrationIt was concentrated
  3. temperaturecooled again to 0° C.
  4. addition250 ml of a normal solution of hydrochloric acid were added
  5. customThe crystallized product was separated out
  6. washwashed with water
  7. customdried
  8. customthen crystallized from an isopropanol—water mixture (1-2)

출처 및 근거

ORD 기록
ord-34f3cad7758b4fcba9a953d40a8281f7
출처 데이터셋
uspto-grants-2001_11
특허 번호
US06313305B1

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