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Acetic Anhydride → HCID 68686254、化合物

HRID 1158886
ノート
印刷プレビュー

反応式

HRID 1158886 の反応式
[CH2:1]([N:8]1[CH2:13][CH2:12][N:11]2[CH:14]=[C:15]([CH:17]=[O:18])[N:16]=[C:10]2[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Mg+2].[Br-].[Br-].[N+:22]([C:25]1[CH:43]=[CH:42][C:28]([CH2:29][O:30][C:31]([C:33]2[N:34]3[C@H:37]([S:38][CH:39]=2)[C@@H:36]([Br:40])[C:35]3=[O:41])=[O:32])=[CH:27][CH:26]=1)([O-:24])=[O:23].[C:44](OC(=O)C)(=[O:46])[CH3:45]>CN(C1C=CN=CC=1)C.C(OCC)(=O)C.CCN(CC)CC.C1COCC1.C(#N)C>[N+:22]([C:25]1[CH:43]=[CH:42][C:28]([CH2:29][O:30][C:31]([C:33]2[N:34]3[C@H:37]([S:38][CH:39]=2)[C:36]([CH:17]([O:18][C:44](=[O:46])[CH3:45])[C:15]2[N:16]=[C:10]4[CH2:9][N:8]([CH2:1][C:2]5[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=5)[CH2:13][CH2:12][N:11]4[CH:14]=2)([Br:40])[C:35]3=[O:41])=[O:32])=[CH:27][CH:26]=1)([O-:24])=[O:23]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

10

反応物 4

HCID 7918Acetic AnhydrideHCID 82241Magnesium BromideHCID 11280588(5R,6S)-6-bromo-7-oxo-4-thia-1-azabicyclo[3.2.0]hept-2-ene-2-carboxylic acid 4-nitrobenzyl esterHCID 21941423HCID 21941423、化合物

生成物 1

HCID 68686254HCID 68686254、化合物

試薬・触媒・溶媒 5

HCID 14284
4-(Dimethylamino)pyridine
触媒
HCID 6342Acetonitrile溶媒
HCID 8028Tetrahydrofuran溶媒
HCID 8471Triethylamine溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
-20 °C

実験手順

7-Benzyl-5,6,7,8-tetrahydroimidazo[1,2-a]pyrazine-2-carbaldehyde (139 mg) was added to the dry acetonitrile (8.7 mL) solution of anhydrous MgBr2 (325 mg) under a nitrogen atmosphere at room temperature. The dry THF solution (8.7 mL) of (5R,6S)-6-bromo-7-oxo-4-thia-1-azabicyclo[3.2.0]hept-2-ene-2-carboxylic acid 4-nitro-benzyl ester (223 mg) was added to the mixture, cooled to −20° C., and Et3N (0.24 mL) was added in one portion. The reaction vessel was covered with foil to exclude light. The reaction mixture was stirred for 5 h at −20° C. and treated with acetic anhydride (0.11 mL) and DMAP (7 mg) in one portion. The reaction mixture was warmed to 0° C. and stirred for 15 h at 0° C. The mixture was diluted with ethyl acetate and washed with 5% citric acid aqueous solution, saturated sodium hydrogen carbonate, water and brine. The organic layer was dried (MgSO4) and filtered. The filtrate was concentrated under reduced pressure. The residue was applied to silica gel column chromatography, then the column was eluted with n-hexane—AcOEt (3/1˜1/1). The titled compound was obtained as two diastereo mixture (80/20, purple amorphous solid, 233 mg, 61%).

後処理

  1. temperatureThe reaction mixture was warmed to 0° C.
  2. stirringstirred for 15 h at 0° C
  3. washwashed with 5% citric acid aqueous solution, saturated sodium hydrogen carbonate, water and brine
  4. dry with materialThe organic layer was dried (MgSO4)
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated under reduced pressure
  7. washthe column was eluted with n-hexane—AcOEt (3/1˜1/1)

出典と根拠

ORDレコード
ord-686bd11fa48e4eb3a2e406d14dc45369
出典データセット
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07812014B2

反応ノート

読み込み中…

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