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

HRID 2102943ノート

反応式

HRID 2102943 の反応式
[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

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒2 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-da1d7bdda921463dadfab30b47f5c4bc
出典データセット
uspto-grants-2009_08
特許番号
US07576099B2

反応ノート

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