Diethyl Ether → 2-Amino-1-(3-methyl-benzo[b]thiophen-2-yl)-ethanone hydrochloride

HRID 1244340ノート

反応式

HRID 1244340 の反応式
Br[CH2:2][C:3]([C:5]1[S:6][C:7]2[CH:14]=[CH:13][CH:12]=[CH:11][C:8]=2[C:9]=1[CH3:10])=[O:4].C1N2CN3CN(C2)C[N:16]1C3.C(OCC)C.[Cl:30]C(Cl)Cl>>[ClH:30].[NH2:16][CH2:2][C:3]([C:5]1[S:6][C:7]2[CH:14]=[CH:13][CH:12]=[CH:11][C:8]=2[C:9]=1[CH3:10])=[O:4]

参加物

5

反応物 4

HCID 3283Diethyl EtherHCID 4101HexamethylenetetramineHCID 6212ChloroformHCID 27798712-Bromo-1-(3-methyl-1-benzothiophen-2-yl)ethan-1-one

生成物 1

HCID 219192252-Amino-1-(3-methyl-benzo[b]thiophen-2-yl)-ethanone hydrochloride収率 93%

実験手順

1.11 g 2-Bromoacetyl-3-methyl-benzothiophene and 0.56 g hexamethylenetetramine in 20 ml trichloromethane were stirred at room temperature for 16 hours. After addition of 15 ml diethylether the mixture was filtered. The solid residue was stirred at room temperature for 3 hours in a mixture of 15 ml methanol and 1.9 ml concentrated hydrochloric acid. The solvents were distilled off and the residue recrystallized from water to yield 0.90 g (93%) 2-amino-1-(3-methyl-benzo[b]thiophen-2-yl)-ethanone hydrochloride as off-white solid; MS (El): m/e=205 (M+, 40%), 175 (M-CH2NH2, 100%), 147 (M-COCH2NH2, 20%).

後処理

  1. filtrationwas filtered
  2. distillationThe solvents were distilled off
  3. customthe residue recrystallized from water

出典と根拠

ORDレコード
ord-b133dc8666bd4fdb88c069a0a2a80a51
出典データセット
uspto-grants-2006_10
特許番号
US07122545B2

反応ノート

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