Phosphorus tribromide → 4-(Bromomethyl)-3,5-dichloropyridine

HRID 629981노트

반응식

HRID 629981 반응식
[Cl:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([Cl:10])[C:7]=1[CH2:8]O.P(Br)(Br)[Br:12]>C(Cl)(Cl)Cl>[Br:12][CH2:8][C:7]1[C:2]([Cl:1])=[CH:3][N:4]=[CH:5][C:6]=1[Cl:10]

참가 물질

4

반응물 2

HCID 24614Phosphorus tribromideHCID 17855219(3,5-Dichloropyridin-4-yl)methanol

생성물 1

HCID 222277664-(Bromomethyl)-3,5-dichloropyridine수율 75.2%

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

To a solution of (3,5-dichloropyridin-4-yl)methanol (470 mg, 2.6 mmol) in anhydrous chloroform (10 mL) was added dropwise a solution of phosphorus tribromide (250 μL, 2.6 mmol) in anhydrous chloroform (2 mL) at 0° C. The mixture was stirred for 1.5 hours at room temperature. The solid was filtered and washed with dichloromethane to afford 4-(bromomethyl)-3,5-dichloropyridine (471 mg, 75% yield), which was used for next step without further purification; 1H NMR (400 MHz, MeOD4): δ 4.76 (s, 2H), 8.63 (s, 2H).

후처리

  1. filtrationThe solid was filtered
  2. washwashed with dichloromethane

출처 및 근거

ORD 기록
ord-c137cb7a66204d47816debf09c55ccd4
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09315521B2

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