ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Potassium tert-butoxide → Diethyl (1S,2S,5R,6S)-2-benzyloxycarbonylamino-4-methylene-bicyclo[3.1.0]hexane-2,6-dicarboxylate

HRID 2037297
ノート
印刷プレビュー

反応式

HRID 2037297 の反応式
[CH3:1]C(C)([O-])C.[K+].[CH2:7]([O:14][C:15]([NH:17][C@@:18]1([C:30]([O:32][CH2:33][CH3:34])=[O:31])[CH2:23][C:22](=O)[C@@H:21]2[C@H:19]1[C@H:20]2[C:25]([O:27][CH2:28][CH3:29])=[O:26])=[O:16])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1>[Br-].C[P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.O1CCCC1.C(OCC)(=O)C>[CH2:7]([O:14][C:15]([NH:17][C@@:18]1([C:30]([O:32][CH2:33][CH3:34])=[O:31])[CH2:23][C:22](=[CH2:1])[C@@H:21]2[C@H:19]1[C@H:20]2[C:25]([O:27][CH2:28][CH3:29])=[O:26])=[O:16])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 23665647Potassium tert-butoxideHCID 86691270HCID 86691270、化合物

生成物 1

HCID 86691272Diethyl (1S,2S,5R,6S)-2-benzyloxycarbonylamino-4-methylene-bicyclo[3.1.0]hexane-2,6-dicarboxylate

試薬・触媒・溶媒 3

HCID 74505Methyltriphenyliphosphonium bromide触媒HCID 8028Tetrahydrofuran溶媒3 回
HCID 8857
Ethyl Acetate
溶媒

実験手順

Under a nitrogen atmosphere, combine methyl-triphenylphosphonium bromide (67.4 g, 184.9 mmol) and tetrahydrofuran (300 mL) with agitation. Add a solution of potassium tert-butoxide (1M) in tetrahydrofuran, 184.9 mL, 184.9 mmol) to the reaction mixture over 15 minutes and stir the resulting slurry at ambient temperature for 3 hours. Dissolve diethyl (1S,2S,5R,6R)-2-benzyloxycarbonylamino-4-oxo-bicyclo[3.1.0]hexane-2,6-dicarboxylate (12.3 kg, 31.6 mol) in tetrahydrofuran (120 mL) and add to the reaction mixture over 1 hour, maintaining the reaction temperature below 30° C. Stir the resulting slurry overnight at ambient temperature, then dilute with ethyl acetate (600 mL) and quench with water (300 mL). After stirring the biphasic mixture for 30 minutes, separate the layers and wash the organics with water (300 mL) followed by 0.25M HCl (300 mL). Dry the organics over Na2SO4, filter, and concentrate in vacuo (45° C.) to afford the crude product as a dark oil (111.0 g). Purify the material by silica gel plug chromatography (1 Kg Kieselgel-60, 4 L 15% EtOAc in heptanes, then 10 L 30% EtOAc in heptanes) to afford the title compound as a clear oil (37.3 g, 87.9% potency, 54.9%). MS (m/z): 388 (M+1).

後処理

  1. temperaturemaintaining the reaction temperature below 30° C
  2. stirringStir the resulting slurry overnight at ambient temperature
  3. customquench with water (300 mL)
  4. stirringAfter stirring the biphasic mixture for 30 minutes
  5. customseparate the layers
  6. washwash the organics with water (300 mL)
  7. dry with materialDry the organics over Na2SO4
  8. filtrationfilter
  9. concentrationconcentrate in vacuo (45° C.)
  10. customto afford the crude product as a dark oil (111.0 g)
  11. customPurify the material by silica gel plug chromatography (1 Kg Kieselgel-60, 4 L 15% EtOAc in heptanes

出典と根拠

ORDレコード
ord-d12d00ab1bab438983860e934fc49770
出典データセット
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08575214B2

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