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Acetic Anhydride → HCID 86607969、化合物

HRID 1158893
ノート
印刷プレビュー

反応式

HRID 1158893 の反応式
[N+:1]([C:4]1[CH:24]=[CH:23][C:7]([CH2:8][O:9][C:10]([N:12]2[CH2:17][CH2:16][N:15]3[N:18]=[C:19]([CH:21]=[O:22])[CH:20]=[C:14]3[CH2:13]2)=[O:11])=[CH:6][CH:5]=1)([O-:3])=[O:2].[Mg+2].[Br-].[Br-].[N+:28]([C:31]1[CH:49]=[CH:48][C:34]([CH2:35][O:36][C:37]([C:39]2[N:40]3[C@H:43]([S:44][CH:45]=2)[C@@H:42]([Br:46])[C:41]3=[O:47])=[O:38])=[CH:33][CH:32]=1)([O-:30])=[O:29].[C:50](OC(=O)C)(=[O:52])[CH3:51]>CN(C1C=CN=CC=1)C.C(OCC)(=O)C.CCN(CC)CC.C1COCC1.C(#N)C>[N+:1]([C:4]1[CH:24]=[CH:23][C:7]([CH2:8][O:9][C:10]([N:12]2[CH2:17][CH2:16][N:15]3[N:18]=[C:19]([CH:21]([O:22][C:50](=[O:52])[CH3:51])[C:42]4([Br:46])[C:41](=[O:47])[N:40]5[C@@H:43]4[S:44][CH:45]=[C:39]5[C:37]([O:36][CH2:35][C:34]4[CH:48]=[CH:49][C:31]([N+:28]([O-:30])=[O:29])=[CH:32][CH:33]=4)=[O:38])[CH:20]=[C:14]3[CH2:13]2)=[O:11])=[CH:6][CH:5]=1)([O-:3])=[O:2]
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 Anhydride2 回HCID 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 11847134HCID 11847134、化合物

生成物 1

HCID 86607969HCID 86607969、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

2-Formyl-6,7-dihydro-4H-pyrazolo[1,5-a]pyrazine-5-carboxylic acid 4-nitrobenzyl ester (2.71 g) was added to the dry acetonitrile (164 mL) solution of anhydrous MgBr2 (cont. 98%) (6.17 g) under a nitrogen atmosphere at room temperature. The dry THF solution (164 mL) of (5R,6S)-6-bromo-7-oxo-4-thia-1-azabicyclo[3.2.0]hept-2-ene-2-carboxylic acid 4-nitrobenzyl ester (cont. 96.5%) (3.27 g) was added to the mixture, cooled to −20° C., and Et3N (cont. 99%) (9.24 mL) was added in one portion. The reaction vessel was covered with foil to exclude light. The reaction mixture was stirred for 1.5 h at −20° C. and treated with acetic anhydride (cont. 97%) (3.19 mL) and DMAP (cont. 99%) (203 mg) in one portion. The reaction mixture was warmed to 0° C. and stirred for 1 h at 0° C. Acetic anhydride (3.19 mL) was added to the solution 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), followed by concentration under reduced pressure. The residue was purified with silica-gel column chromatography three times (n-hexane-AcOEt (1/1 to 2/3), CHCl3-acetone (29/1 to 19/1) and CHCl3-acetone (29/1)). The titled compound was obtained as yellow amorphous (diastereo-mixture (64:36), 3.30 g, 53%).

後処理

  1. temperatureThe reaction mixture was warmed to 0° C.
  2. stirringstirred for 1 h at 0° C
  3. stirringstirred for 15 h at 0° C
  4. washwashed with 5% citric acid aqueous solution, saturated sodium hydrogen carbonate, water and brine
  5. dry with materialThe organic layer was dried (MgSO4)
  6. concentrationfollowed by concentration under reduced pressure
  7. customThe residue was purified with silica-gel column chromatography three times (n-hexane-AcOEt (1/1 to 2/3), CHCl3-acetone (29/1 to 19/1) and CHCl3-acetone (29/1))

出典と根拠

ORDレコード
ord-8d4adb2d5aa848c5990ea34162a84507
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

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