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Sodium borohydride → HCID 67572167, 화합물

HRID 1417546
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HRID 1417546 반응식
[Br:1][C:2]1[C:7]([CH3:8])=[C:6]([N+:9]([O-])=O)[CH:5]=[CH:4][C:3]=1[S:12][CH3:13].[BH4-].[Na+]>CO.CCOCC.C([O-])(=O)C.[Cu+2].C([O-])(=O)C>[Br:1][C:2]1[C:7]([CH3:8])=[C:6]([NH2:9])[CH:5]=[CH:4][C:3]=1[S:12][CH3:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 4311764Sodium borohydrideHCID 67571039HCID 67571039, 화합물

생성물 1

HCID 67572167HCID 67572167, 화합물수율 92.1%

시약·촉매·용매 3

HCID 8895Cupric acetate촉매HCID 887Methanol용매2회HCID 3283Diethyl Ether용매

실험 절차

To a solution of 2-bromo-4-nitro-methylthioanisole (450 mg, 1.81 mmol) in 45 mL of MeOH was added a suspension of copper(11) acetate (85 mg, 0.47 mmol) in 9 mL of MeOH. Sodium borohydride (300 mg, 7.9 mmol) was added as a solid over 0.5 h. The reaction was diluted with Et2O, washed with NaHCO3, dried with Na2SO4, filtered, and conc. to give 387 mg of the title compound. MS:m/e=218 (M+1) 1H NMR (400 Mhz, CDCl3): δ 2.35 (s, 3H), 6.62 (dd, 1H), 6.94 (d, 1H), 7.08 (d, 1H)

후처리

  1. washwashed with NaHCO3
  2. dry with materialdried with Na2SO4
  3. filtrationfiltered

출처 및 근거

ORD 기록
ord-732119a0e9e04a1f8458c7a5d8ad476b
출처 데이터셋
uspto-grants-1999_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05877191

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