Phenyltrimethylammonium bromide dibromide → HCID 22474281, 화합물

HRID 2183617노트

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HRID 2183617 반응식
[Cl:1][C:2]1[C:10]2[CH:9]=[C:8]([C:11](=[O:14])[CH2:12][CH3:13])[S:7][C:6]=2[CH:5]=[CH:4][CH:3]=1.[Br-:15].[Br-].[Br-].C1([N+](C)(C)C)C=CC=CC=1.C1([N+](C)(C)C)C=CC=CC=1.C1([N+](C)(C)C)C=CC=CC=1>O1CCCC1>[Br:15][CH:12]([CH3:13])[C:11]([C:8]1[S:7][C:6]2[CH:5]=[CH:4][CH:3]=[C:2]([Cl:1])[C:10]=2[CH:9]=1)=[O:14]

참가 물질

4

반응물 2

HCID 17977687Phenyltrimethylammonium bromide dibromideHCID 224738541-(4-Chlorobenzo[b]thien-2-yl)-1-propanone

생성물 1

HCID 22474281HCID 22474281, 화합물수율 236.8%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of 1-(4-chlorobenzo[b]thiophen-2-yl)propan-1-one (1.65 g), phenyltrimethylammonium tribromide (2.76 g) and tetrahydrofuran (20 ml) was stirred under nitrogen for 18.5 hours, then it was filtered and diluted with water (200 ml). The product was extracted into dichloromethane (3×40 ml), the combined extracts were dried (MgSO4) and the solvents were removed in vacuo. The residue was purified by flash chromatography over silica using dichloromethane as eluant. Appropriate fractions were combined and the solvents removed in vacuo to leave 2-bromo-1-(4-chlorobenzo[b]thiophen-2-yl)propan-1-one (3.06 g) as a pale yellow solid, m.p. 104-106° C.

후처리

  1. filtrationit was filtered
  2. additiondiluted with water (200 ml)
  3. extractionThe product was extracted into dichloromethane (3×40 ml)
  4. dry with materialthe combined extracts were dried (MgSO4)
  5. customthe solvents were removed in vacuo
  6. customThe residue was purified by flash chromatography over silica
  7. customthe solvents removed in vacuo

출처 및 근거

ORD 기록
ord-148214b3cf8749c288f2685d326a55db
출처 데이터셋
uspto-grants-2005_05
특허 번호
US06900216B2

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