Ammonia → 4-(Aminomethyl)-2-methoxybenzonitrile

HRID 378327노트

반응식

HRID 378327 반응식
Br[CH2:2][C:3]1[CH:10]=[CH:9][C:6]([C:7]#[N:8])=[C:5]([O:11][CH3:12])[CH:4]=1.CO.[NH3:15].N.CO>C(Cl)Cl>[NH2:15][CH2:2][C:3]1[CH:10]=[CH:9][C:6]([C:7]#[N:8])=[C:5]([O:11][CH3:12])[CH:4]=1

참가 물질

6

반응물 4

HCID 222AmmoniaHCID 887MethanolHCID 21705897Ammonia methanolHCID 219850074-(Bromomethyl)-2-methoxybenzonitrile

생성물 1

HCID 224761464-(Aminomethyl)-2-methoxybenzonitrile

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

2.5 g of the bromide (b) were introduced into 10 ml of MeOH, and NH3 was passed in during dropwise addition of 38 ml of conc. ammonia/MeOH 1:1. After 2 h, the solvent was stripped off, the product was taken up in DCM and washed with water, and the organic phase was dried over Na2SO4. The product was precipitated as hydrochloride with ethereal HCl. 1H-NMR (DMSO-d6, δ in ppm): 8.6 (broad signal, NH3+), 7.79 (1H), 7.55 (1H), 7.20 (1H), 4.10 (s, 2H), 3.93 (s, 3H)

후처리

  1. washwashed with water
  2. dry with materialthe organic phase was dried over Na2SO4
  3. customThe product was precipitated as hydrochloride with ethereal HCl

출처 및 근거

ORD 기록
ord-5a0e744ad4f649a29fca5093a502c2f2
출처 데이터셋
uspto-grants-2000_02
특허 번호
US06030972

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