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Bromine → 2-bromo-4H,5H,6H,7H-thieno(2,3-c)pyridine hydrobromide

HRID 1505933
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반응식

HRID 1505933 반응식
[Br:1]Br.Cl.[S:4]1[C:8]2[CH2:9][NH:10][CH2:11][CH2:12][C:7]=2[CH:6]=[CH:5]1>C(O)(=O)C>[BrH:1].[Br:1][C:5]1[S:4][C:8]2[CH2:9][NH:10][CH2:11][CH2:12][C:7]=2[CH:6]=1
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참가 물질

4

반응물 2

HCID 24408BromineHCID 250673334,5,6,7-Tetrahydrothieno(2,3-c)pyridine--hydrogen chloride (1/1)

생성물 1

HCID 670276802-bromo-4H,5H,6H,7H-thieno(2,3-c)pyridine hydrobromide수율 176.8%

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

실험 절차

A solution of bromine (139 mg, 0.87 mmol) in acetic acid (0.5 mL) was added to a solution of 4,5,6,7-tetrahydrothieno[2,3-c]pyridine hydrochloride (150 mg, 0.85 mmol) in acetic acid (3 mL) and the mixture left to stir at ambient temperature for 1.5 h. The resultant precipitate was collected by filtration, washed with diethyl ether and left to air dry to afford the title compound as an off-white solid (230 mg, 90%). NMR (DMSO-D6, 300 MHz): 9.19 (s, 2H), 7.09 (s, 1H), 4.29-4.26 (m, 2H), 2.86-2.78 (m, 2H), 2.52-2.48 (m, 2H). LCMS (Method B): RT=1.65 min, M+H+=218/220.

후처리

  1. waitthe mixture left
  2. filtrationThe resultant precipitate was collected by filtration
  3. washwashed with diethyl ether
  4. waitleft to air
  5. customdry

출처 및 근거

ORD 기록
ord-4a407b8b3ecf45a5bfea946ececea87b
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09216980B2

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