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Ammonia → 3-(3-Bromo-4-fluorophenyl)propanimidamide hydrochloride

HRID 705800
ノート
印刷プレビュー

反応式

HRID 705800 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH2:9][CH2:10][C:11]#[N:12])[CH:5]=[CH:6][C:7]=1[F:8].CO.C([Cl:18])(=O)C.[NH3:19]>C1(C)C=CC=CC=1>[ClH:18].[Br:1][C:2]1[CH:3]=[C:4]([CH2:9][CH2:10][C:11](=[NH:19])[NH2:12])[CH:5]=[CH:6][C:7]=1[F:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 222AmmoniaHCID 887MethanolHCID 6367Acetyl chlorideHCID 534343013-(3-Bromo-4-fluorophenyl)propanenitrile

生成物 1

HCID 677757593-(3-Bromo-4-fluorophenyl)propanimidamide hydrochloride収率 93%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To a solution of 3-(3-bromo-4-fluorophenyl)propanenitrile (5.0 g, 21.05 mmol) in toluene (20 mL) and methanol (6.32 mL, 156 mmol) at 0° C. was added acetyl chloride (7.51 mL, 105 mmol) dropwise over 5 min. The reaction mixture was allowed to warm to room temperature and stirred for 2 h. The mixture was cooled to 0° C. by an ice bath, to which ammonia (30.1 mL, 210 mmol) was added dropwise. The reaction mixture was stirred at room temperature overnight. The mixture was filtered, and the filtrate was concentrated to give a crude product. Recrystallization from toluene/methanol (1:1) then afforded the title compound as a white solid (5.2 g, 93% yield). LCMS: rt=1.18 min, [M+H+]=245

後処理

  1. additionwas added dropwise
  2. stirringThe reaction mixture was stirred at room temperature overnight
  3. filtrationThe mixture was filtered
  4. concentrationthe filtrate was concentrated
  5. customto give a crude product
  6. customRecrystallization from toluene/methanol (1:1)

出典と根拠

ORDレコード
ord-d19e01cfc92548939426b0981488eb79
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09174968B2

反応ノート

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