Ammonia → N'-(4-bromophenyl)-2-chloro-6-fluorobenzenecarbohydrazonamide

HRID 59225

反応式

HRID 59225 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][N:9]=[C:10](Cl)[C:11]2[C:16]([F:17])=[CH:15][CH:14]=[CH:13][C:12]=2[Cl:18])=[CH:4][CH:3]=1.[NH3:20]>C1COCC1>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][N:9]=[C:10]([C:11]2[C:16]([F:17])=[CH:15][CH:14]=[CH:13][C:12]=2[Cl:18])[NH2:20])=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 222AmmoniaHCID 131733232N-(4-bromophenyl)-2-chloro-6-fluorobenzenecarbohydrazonoyl chloride

生成物 1

HCID 117965458N'-(4-bromophenyl)-2-chloro-6-fluorobenzenecarbohydrazonamide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
2.5 °C

実験手順

To a cold solution of N-(4-bromophenyl)-2-chloro-6-fluorobenzenecarbohydrazonoyl chloride (0.070 g, 0.267 mmol) in dry THF was added aq. ammonia. The reaction mass was stirred at 0-5° C. for 2-3 h. The reaction mass was quenched in water, neutralized with dilute acetic acid and extracted with DCM. The organic layer was dried over anhydrous sodium sulphate and concentrated to afford 0.040 g of the desired product. 1H NMR (300 MHz, DMSO d6): δ 6.29 (br s, 2H), 6.80 (d, J=8.4 Hz, 2H), 7.24 (d, J=9.3 Hz, 2H), 7.28-7.50 (m, 3H), 8.33 (s, 1H).

後処理

  1. customThe reaction mass was quenched in water
  2. extractionextracted with DCM
  3. dry with materialThe organic layer was dried over anhydrous sodium sulphate
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-e3b3e7e8935b47088e554424e5b52271
出典データセット
uspto-grants-2016_09
特許番号
US09439890B2

関連ノート

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