Ammonia → 4-(Aminomethyl)-2-methoxybenzonitrile

HRID 1278926노트

반응식

HRID 1278926 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-9d67b28124344561a17a4f48759d32e0
출처 데이터셋
uspto-grants-2002_09
특허 번호
US06444817B1

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