Ammonium Hydroxide → 2-((Cyclopropylmethoxy)methyl)-2,3-dihydrobenzo[b][1,4]dioxin-6-amine

HRID 2102943노트

반응식

HRID 2102943 반응식
[CH:1]1([CH2:4][O:5][CH2:6][CH:7]2[O:12][C:11]3[CH:13]=[CH:14][C:15]([N+:17]([O-])=O)=[CH:16][C:10]=3[O:9][CH2:8]2)[CH2:3][CH2:2]1.S(S([O-])=O)([O-])=O.[Na+].[Na+].[NH4+].[OH-]>O1CCOCC1.O>[CH:1]1([CH2:4][O:5][CH2:6][CH:7]2[O:12][C:11]3[CH:13]=[CH:14][C:15]([NH2:17])=[CH:16][C:10]=3[O:9][CH2:8]2)[CH2:3][CH2:2]1

참가 물질

6

반응물 3

HCID 14923Ammonium HydroxideHCID 24489Sodium DithioniteHCID 687021632-((Cyclopropylmethoxy)methyl)-2,3-dihydro-6-nitrobenzo[b][1,4]dioxine

생성물 1

HCID 590206732-((Cyclopropylmethoxy)methyl)-2,3-dihydrobenzo[b][1,4]dioxin-6-amine

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매2회

실험 절차

2-((Cyclopropylmethoxy)methyl)-2,3-dihydro-6-nitrobenzo[b][1,4]dioxine (0.33 g, 0.0012 mol) was dissolved in 20 mL dioxane. Sodium dithionite (2.2 g, 0.013 mol) was suspended in water (4 mL) and NH4OH (2 mL) and then added to the dioxane solution. The reaction was stirred at room temp for 6 hrs. The mixture was filtered through filter paper and the filtrate concentrated under vacuum to a white solid. The solid was suspended in 10% EtOAc/hexanes and filtered. The filtrate was concentrated to a white solid and used for the next reaction without further purification. Yield of the title compound is 0.29 g (98%). m/z=235.8 (M+1).

후처리

  1. filtrationThe mixture was filtered
  2. filtrationthrough filter paper
  3. concentrationthe filtrate concentrated under vacuum to a white solid
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated to a white solid
  6. customused for the next reaction without further purification

출처 및 근거

ORD 기록
ord-da1d7bdda921463dadfab30b47f5c4bc
출처 데이터셋
uspto-grants-2009_08
특허 번호
US07576099B2

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