Ammonia → 4-(Aminomethyl)-2-methoxybenzonitrile

HRID 378327ノート

反応式

HRID 378327 の反応式
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

参加物

6

反応物 4

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

生成物 1

HCID 224761464-(Aminomethyl)-2-methoxybenzonitrile

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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)

後処理

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

出典と根拠

ORDレコード
ord-5a0e744ad4f649a29fca5093a502c2f2
出典データセット
uspto-grants-2000_02
特許番号
US06030972

反応ノート

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