Sodium Azide → HCID 16748734, 화합물

HRID 457574

반응식

HRID 457574 반응식
[Br:1][C:2]1[CH:3]=[C:4]([CH:9]=[CH:10][CH:11]=1)[C:5](=[O:8])[CH2:6]Br.[N-:12]=[N+:13]=[N-:14].[Na+]>CO>[Br:1][C:2]1[CH:3]=[C:4]([CH:9]=[CH:10][CH:11]=1)[C:5](=[O:8])[CH2:6][N:12]=[N+:13]=[N-:14]

참가 물질

4

반응물 2

HCID 33557Sodium AzideHCID 5195852-Bromo-1-(3-bromophenyl)ethan-1-one

생성물 1

HCID 16748734HCID 16748734, 화합물수율 99.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 20.2 g (73 mmol) of 3-bromophenacyl bromide and 5.42 g (83 mmol) of sodium azide was stirred at RT for 90 min in methanol. The solvent was removed under reduced pressure and the crude product was partitioned between ethyl acetate (200 ml) and water (100 mL). The organic layer was separated, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to afford the title compound (17.4 g, 99%) as a light yellow solid. 1H NMR (400 MHz, d6-DMSO): δ 8.10 (d, J=1.0, 1H), 7.90–7.97 (m, 2H), 7.22 (t, J=7.9, 1H), 4.93 (s, 2H).

후처리

  1. customThe solvent was removed under reduced pressure
  2. customthe crude product was partitioned between ethyl acetate (200 ml) and water (100 mL)
  3. customThe organic layer was separated
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-04496d367c7b4f678864836d4b3ee3b1
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07189712B2

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