Hydrochloric Acid → (2-Bromo-phenyl)-piperazin-1-yl-methanone hydrochloride

HRID 1665585ノート

反応式

HRID 1665585 の反応式
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14](=[O:22])[C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[Br:21])[CH2:10][CH2:9]1)=O)(C)(C)C.[ClH:23]>>[ClH:23].[Br:21][C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=1[C:14]([N:11]1[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]1)=[O:22]

参加物

3

反応物 2

HCID 313Hydrochloric AcidHCID 17952334Tert-butyl 4-(2-bromobenzoyl)piperazine-1-carboxylate

生成物 1

HCID 66625832(2-Bromo-phenyl)-piperazin-1-yl-methanone hydrochloride収率 95%

実験手順

HCl (50 mL) was added to 4-(2-bromo-benzoyl)-piperazine-1-carboxylic acid tert-butyl ester (9 g, 24.4 mmol) at 0° C. The resulting mixture was stirred for 4 hours, then concentrated. The resulting residue was washed with 1% MeOH in ethyl acetate and dried under reduced pressure to afford 7.1 g (95%) of (2-bromo-phenyl)-piperazin-1-yl-methanone hydrochloride salt, LCMS: 306.6 (M+1)+, 86.8%, 1H NMR: (DMSO-d6): δ 9.6 (s, 2H), 7.7 (d, 1H), 7.45 (m, 3H), 4.0 (m, 1H), 3.76 (m, 1H), 3.18 (bs, 2H), 3.06 (bs, 2H).

後処理

  1. concentrationconcentrated
  2. washThe resulting residue was washed with 1% MeOH in ethyl acetate
  3. customdried under reduced pressure

出典と根拠

ORDレコード
ord-91746ebd5bf747bdaee3119c1a5c5db1
出典データセット
uspto-grants-2011_10
特許番号
US08039463B2

反応ノート

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