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Hydrochloric Acid → (2-Bromo-6-fluorophenyl)hydrazine hydrochloride

HRID 341082
ノート
印刷プレビュー

反応式

HRID 341082 の反応式
[Br:1][C:2]1[CH:8]=[CH:7][CH:6]=[C:5]([F:9])[C:3]=1[NH2:4].[ClH:10].[N:11]([O-])=O.[Na+]>[OH-].[Na+]>[ClH:10].[Br:1][C:2]1[CH:8]=[CH:7][CH:6]=[C:5]([F:9])[C:3]=1[NH:4][NH2:11]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric Acid2 回HCID 27829402-Bromo-6-fluoroanilineHCID 23668193Sodium Nitrite

生成物 1

HCID 2783128(2-Bromo-6-fluorophenyl)hydrazine hydrochloride

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒2 回

反応条件

温度
0 °C

実験手順

2-Bromo-6-fluoroaniline (2.0 g, 11 mmol) was dissolved in hydrochloric acid (7.0 mL, 12 N aqueous, 84 mmol, 8 equiv) and cooled to 0° C. An aqueous solution (10 mL) of sodium nitrite (0.80 g, 12 mmol, 1.1 equiv) was added dropwise over 30 minutes via additional funnel and the mixture was stirred for an additional 30 minutes at 0° C. A hydrochloric acid solution (10 mL, 12 N aqueous) of stannous(II) chloride dihydrate (7.1 g, 32 mmol, 3 equiv) was then added to the mixture over 45 minutes via additional funnel and the mixture was stirred for an additional 1 hour at 0° C. To the mixture, sodium hydroxide (30 mL, 1 M aqueous) was added slowly until basic by pH paper. The mixture was warmed to ambient temperature, poured into sodium hydroxide (50 mL, 25% aqueous) and the aqueous layer was extracted with diethyl ether (3×250 mL). The combined organic extracts were dried with sodium sulfate, filtered and partially concentrated in vacuo. The residue was taken up in diethyl ether and treated with gaseous hydrochloric acid. The solid was filtered and washed with diethyl ether, providing the titled compound as a white solid.

後処理

  1. stirringthe mixture was stirred for an additional 1 hour at 0° C
  2. temperatureThe mixture was warmed to ambient temperature
  3. extractionthe aqueous layer was extracted with diethyl ether (3×250 mL)
  4. dry with materialThe combined organic extracts were dried with sodium sulfate
  5. filtrationfiltered
  6. concentrationpartially concentrated in vacuo
  7. additiontreated with gaseous hydrochloric acid
  8. filtrationThe solid was filtered
  9. washwashed with diethyl ether

出典と根拠

ORDレコード
ord-8c2649a3427444b19361631e0b7e6c13
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08895580B2

反応ノート

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