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Hydrazine hydrate (1:1) → HCID 12782786、化合物

HRID 1155000
ノート
印刷プレビュー

反応式

HRID 1155000 の反応式
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N+:8]([O-])=[O:9].O.NN>[Rh].O1CCCC1>[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[NH:8][OH:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 24654Hydrazine hydrate (1:1)2 回HCID 738951-Fluoro-2-nitrobenzene

生成物 1

HCID 12782786HCID 12782786、化合物

試薬・触媒・溶媒 2

HCID 23948Rhodium触媒2 回HCID 8028Tetrahydrofuran溶媒

実験手順

0.5 g of a commercial rhodium catalyst (5% on charcoal) was added to a stirred mixture of 25 g of 2-fluoronitrobenzene and 250 ml of tetrahydrofuran at room temperature. Then 16.5 g of hydrazine hydrate was added, drop-by-drop, to the stirred mixture, maintained at 15°-20° C. After 20 minutes, another 0.5 g of the rhodium catalyst was added, then another 2 g of hydrazine hydrate was added. The mixture was stirred at 15°-20° C. for 2 hours, then filtered through Celite. The filtrate was extracted with ether, the extract was washed with water, and dried (MgSO4) and the solvent was evaporated. The residue was triturated with ether and hexane, and kept cold until filtered. The filter cake was washed with cold hexane and air-dried to give N-(2-fluorophenyl)hydroxylamine (1B) as a colorless solid, mp: 70°-71° C. It is moderately unstable at room temperature.

後処理

  1. temperaturedrop-by-drop, to the stirred mixture, maintained at 15°-20° C
  2. filtrationfiltered through Celite
  3. extractionThe filtrate was extracted with ether
  4. washthe extract was washed with water
  5. dry with materialdried (MgSO4)
  6. customthe solvent was evaporated
  7. customThe residue was triturated with ether and hexane
  8. filtrationuntil filtered
  9. washThe filter cake was washed with cold hexane
  10. customair-dried

出典と根拠

ORDレコード
ord-139ed7e8459445f09882dc4d8b206750
出典データセット
uspto-grants-1981_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04299778

反応ノート

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