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Diethyl Pyrocarbonate → HCID 57846915、化合物

HRID 735756
ノート
印刷プレビュー

反応式

HRID 735756 の反応式
[C:1]1([C@@H:7]2[C@@H:16]3[CH2:17][CH2:18][NH:19][C@@H:15]3[C:14]3[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=3[NH:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:20]([NH:28][C@@H:29]1[CH2:34][CH2:33][CH2:32][CH2:31][C@@H:30]1[C:35](O)=[O:36])(=[O:27])[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.C(N(CC)CC)C.CCOC(OC(OCC)=O)=O.C(=O)([O-])O.[Na+]>O1CCCC1.C(#N)C>[C:1]1([C@H:7]2[C@H:16]3[CH2:17][CH2:18][N:19]([C:35]([C@H:30]4[CH2:31][CH2:32][CH2:33][CH2:34][C@H:29]4[NH:28][C:20](=[O:27])[C:21]4[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=4)=[O:36])[C@H:15]3[C:14]3[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=3[NH:8]2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 3051Diethyl PyrocarbonateHCID 8471TriethylamineHCID 516892Sodium BicarbonateHCID 1268229(+)-cis-2-Benzamidocyclohexanecarboxylic AcidHCID 57846973HCID 57846973、化合物

生成物 1

HCID 57846915HCID 57846915、化合物収率 62%

試薬・触媒・溶媒

2
HCID 6342Acetonitrile溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a mixture of (3aR*,4S*,9bS)-4-phenyl-2,3,3a,4,5,9b-hexahydro-1H-pyrrolo[3,2-c]quinoline (620 mg, 2.47 mmol), (1S,2R)-2-(benzoylamino)cyclohexanecarboxylic acid (671 mg, 2.7 mmol), triethylamine (0.72 ml, 5.2 mmol), acetonitrile (17 ml) and tetrahydrofuran (17 ml) was added dropwise DEPC (440 mg, 2.7 mmol) under ice-cooling, and the mixture was stirred for 10 min. The mixture was allowed to return to room temperature and the mixture was stirred for 1 hr. Saturated aqueous sodium hydrogen carbonate solution was added to the reaction mixture and the mixture was extracted with ethyl acetate. The extract was dried (over anhydrous Na2 SO4), and the solvent was evaporated. The residue was subjected to column chromatography using silica gel (30 g), and eluted with hexane-ethyl acetate (9:1-7:3, v/v) to give the title compound (735 mg, 62%) as an amorphous form.

後処理

  1. temperaturecooling
  2. customto return to room temperature
  3. stirringthe mixture was stirred for 1 hr
  4. extractionthe mixture was extracted with ethyl acetate
  5. customThe extract was dried (over anhydrous Na2 SO4)
  6. customthe solvent was evaporated
  7. washeluted with hexane-ethyl acetate (9:1-7:3

出典と根拠

ORDレコード
ord-a27f8b7519c04102927ce70b765e3671
出典データセット
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07592453B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート