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4-Methylmorpholine → 2-Bromo-5-fluoro-4-[2-methyl-1-(2-nitro-benzenesulfonyl)-aziridin-2-yl]-pyridine

HRID 538345
ノート
印刷プレビュー

反応式

HRID 538345 の反応式
[Br:1][C:2]1[CH:7]=[C:6]([C:8]2([CH3:11])[CH2:10][NH:9]2)[C:5]([F:12])=[CH:4][N:3]=1.P(C1C=CC=CC=1)(C1C=CC=CC=1)(C1C=CC=CC=1)=O.[N+:33]([C:36]1[CH:41]=[CH:40][CH:39]=[CH:38][C:37]=1[S:42](Cl)(=[O:44])=[O:43])([O-:35])=[O:34].CN1CCOCC1>C1COCC1.O>[Br:1][C:2]1[CH:7]=[C:6]([C:8]2([CH3:11])[CH2:10][N:9]2[S:42]([C:37]2[CH:38]=[CH:39][CH:40]=[CH:41][C:36]=2[N+:33]([O-:35])=[O:34])(=[O:43])=[O:44])[C:5]([F:12])=[CH:4][N:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 79724-MethylmorpholineHCID 13097Triphenylphosphine OxideHCID 155402-Nitrobenzenesulfonyl chlorideHCID 866680542-Bromo-5-fluoro-4-(2-methyl-aziridin-2-yl)-pyridine

生成物 1

HCID 866680552-Bromo-5-fluoro-4-[2-methyl-1-(2-nitro-benzenesulfonyl)-aziridin-2-yl]-pyridine

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of crude 2-bromo-5-fluoro-4-(2-methyl-aziridin-2-yl)-pyridine (3.17 g as a 45% mixture with Ph3PO, 6.17 mmol) and 2-nitrobenzene-1-sulfonyl chloride (1.368 g, 6.17 mmol) in THF (23.15 mL) and H2O (7.72 mL) was added N-methylmorpholine and the reaction mixture was stirred at rt for 1.5 h. Alox neutral (2-3 spatula) was added and the reaction mixture was filtered through celite, washed with DCM and the filtrates were diluted with DCM and 1M aq. NaHCO3 soln. The phases were separated and the aq. phase was reextracted twice with DCM. The combined org. phases were dried over Na2SO4 and concentrated. Flash chromatography on silica gel (heptane:EtOAc 4:1 to 3:1) followed by recrystallization from EtOAc/hexane yielded the title compound as a colourless solid. HPLC RtH4=1.11 min; ESIMS: 416, 418 [(M+H)+]; 1H NMR (400 MHz, CDCl3): δ 8.31-8.30 (m, 1H), 8.23 (d, 1H), 7.86-7.77 (m, 3H), 7.68 (d, 1H), 3.28 (s, 1H), 2.78 (s, 1H), 2.09 (s, 3H).

後処理

  1. additionAlox neutral (2-3 spatula) was added
  2. filtrationthe reaction mixture was filtered through celite
  3. washwashed with DCM
  4. additionthe filtrates were diluted with DCM and 1M aq. NaHCO3 soln
  5. customThe phases were separated
  6. dry with materialphases were dried over Na2SO4
  7. concentrationconcentrated
  8. customFlash chromatography on silica gel (heptane:EtOAc 4:1 to 3:1) followed by recrystallization from EtOAc/hexane

出典と根拠

ORDレコード
ord-cb961b84637a4557901477a6bf53a1e8
出典データセット
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08865712B2

反応ノート

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