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

HRID 1098190ノート

反応式

HRID 1098190 の反応式
Cl.O1CCOCC1.[Br:8][C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([Cl:15])[C:10]=1[N:16](C(OC(C)(C)C)=O)[NH:17]C(OC(C)(C)C)=O>CC(O)C>[ClH:15].[Br:8][C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([Cl:15])[C:10]=1[NH:16][NH2:17]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 57438660Di-tert-butyl 1-(2-bromo-6-chlorophenyl)hydrazine-1,2-dicarboxylate

生成物 1

HCID 57504666(2-Bromo-6-chlorophenyl)hydrazine hydrochloride収率 162.1%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

反応条件

温度
60 °C

実験手順

4M Hydrogen chloride in dioxane (28.2 mL, 112.64 mmol) was added to di-tert-butyl 1-(2-bromo-6-chlorophenyl)hydrazine-1,2-dicarboxylate (Intermediate AH1) (9.5 g, 22.53 mmol) in iPrOH (30 mL) at ambient temperature. The resulting solution was heated to 60° C. and stirred for 20 minutes. The reaction mixture was allowed to cool to ambient temperature. A solid was filtered off, and dried under vacuum to afford the product (4.71 g). 1H NMR (400 MHz, DMSO) d 6.97 (1H, s), 7.06 (1H, t), 7.41 (1H, dd), 7.52 (1H, dd), 9.83 (3H, s). m/z M.+=220; GC-MS tR=10.419 min.

後処理

  1. temperatureto cool to ambient temperature
  2. filtrationA solid was filtered off
  3. customdried under vacuum

出典と根拠

ORDレコード
ord-3d847cca13394258abe102013ad40e90
出典データセット
uspto-grants-2012_03
特許番号
US08143263B2

反応ノート

読み込み中…