Hydrazine hydrate (1:1) → 2,6-Dichloro-4-methoxy-benzylamine hydrochloride

HRID 1670814노트

반응식

HRID 1670814 반응식
[Cl:1][C:2]1[CH:19]=[C:18]([O:20][CH3:21])[CH:17]=[C:16]([Cl:22])[C:3]=1[CH2:4][N:5]1C(=O)C2C(=CC=CC=2)C1=O.O.NN>C(O)C>[ClH:1].[Cl:1][C:2]1[CH:19]=[C:18]([O:20][CH3:21])[CH:17]=[C:16]([Cl:22])[C:3]=1[CH2:4][NH2:5]

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 673536412-(2,6-Dichloro-4-methoxy-benzyl)-isoindole-1,3-dione

생성물 1

HCID 673555502,6-Dichloro-4-methoxy-benzylamine hydrochloride수율 166.3%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Treat a solution of 2-(2,6-Dichloro-4-methoxy-benzyl)-isoindole-1,3-dione (2.74 g, 8.18 mmol) in ethanol with hydrazine hydrate (0.61 g, 12.27 mmol) at 70° C. for 12 hours. Cool the reaction and filter the precipitate. Concentrate the filtrate and partition the residue with ethyl acetate and water. After drying the organic layer over sodium sulfate, filter and concentrate under vacuum. To the residue, add ethyl acetate (20 mL) and HCl (4 N in dioxane, 5 mL). Collect the white crystal by filtration and air dry to afford 1.65 g (84%) of the title compound. MS (m/z): 242 (M+H)+.

후처리

  1. temperatureCool
  2. customthe reaction
  3. filtrationfilter the precipitate
  4. concentrationConcentrate the filtrate
  5. custompartition the residue with ethyl acetate and water
  6. dry with materialAfter drying the organic layer over sodium sulfate
  7. filtrationfilter
  8. concentrationconcentrate under vacuum
  9. additionTo the residue, add ethyl acetate (20 mL) and HCl (4 N in dioxane, 5 mL)
  10. customCollect the white crystal
  11. filtrationby filtration and air
  12. customdry

출처 및 근거

ORD 기록
ord-ba017527473d4b31accd5399dc407ed1
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07994176B2

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