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

HRID 1244340노트

반응식

HRID 1244340 반응식
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]

참가 물질

5

반응물 4

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

생성물 1

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

실험 절차

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%).

후처리

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

출처 및 근거

ORD 기록
ord-b133dc8666bd4fdb88c069a0a2a80a51
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07122545B2

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