Ammonia → 4-Bromo-2-fluorobenzimidamide hydrochloride

HRID 1530481ノート

反応式

HRID 1530481 の反応式
[ClH:1].C(O[C:5](=[NH:14])[C:6]1[CH:11]=[CH:10][C:9]([Br:12])=[CH:8][C:7]=1[F:13])C.[NH3:15]>>[ClH:1].[Br:12][C:9]1[CH:10]=[CH:11][C:6]([C:5]([NH2:14])=[NH:15])=[C:7]([F:13])[CH:8]=1

参加物

3

反応物 2

HCID 222AmmoniaHCID 670507354-Bromo-2-fluoro-benzimidic acid ethyl ester hydrochloride

生成物 1

HCID 534078914-Bromo-2-fluorobenzimidamide hydrochloride収率 100%

実験手順

A mixture of 4-bromo-2-fluoro-benzimidic acid ethyl ester hydrochloride (20.3 g, 72 mmol) in IMS (250 mL) at 0-5° C. was saturated with NH3 (gas), and the flask sealed before allowing to warm to RT and stirring for 18 h. Solvent was removed in vacuo and the residue triturated in diethyl ether to give 4-Bromo-2-fluoro-benzamidine hydrochloride as a white solid (18.1 g, 100%). 1H NMR δ (ppm) (DMSO-d6): 9.26 (4H, s), 7.92-7.87 (1H, m), 7.71-7.62 (2H, m).

後処理

  1. customthe flask sealed
  2. customSolvent was removed in vacuo
  3. customthe residue triturated in diethyl ether

出典と根拠

ORDレコード
ord-885234a4e94d43f58288a762ffb98d1d
出典データセット
uspto-grants-2015_07
特許番号
US09090628B2

反応ノート

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