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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
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Water → HCID 90295830、化合物

HRID 1050200
ノート
印刷プレビュー

反応式

HRID 1050200 の反応式
[O:1]=[C:2]1[N:6]2[C:7]3[CH:14]=[CH:13][C:12]([N:15]4[CH2:20][CH2:19][O:18][CH2:17][C:16]4=[O:21])=[CH:11][C:8]=3[O:9][CH2:10][C@H:5]2[C@@H:4]([CH2:22]CS([O-])(=O)=O)[O:3]1.[K].[C:29]1(=[O:39])[NH:33][C:32](=[O:34])[C:31]2=[CH:35][CH:36]=[CH:37][CH:38]=[C:30]12.C(Cl)Cl.CO.O>CN(C=O)C>[O:1]=[C:2]1[N:6]2[C:7]3[CH:14]=[CH:13][C:12]([N:15]4[CH2:20][CH2:19][O:18][CH2:17][C:16]4=[O:21])=[CH:11][C:8]=3[O:9][CH2:10][C@H:5]2[C@H:4]([CH2:22][N:33]2[C:29](=[O:39])[C:30]3[C:31](=[CH:35][CH:36]=[CH:37][CH:38]=3)[C:32]2=[O:34])[O: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

6

反応物 4

HCID 962WaterHCID 21226129Dichloromethane methanolHCID 24194345Phthalimide potassium saltHCID 131736049HCID 131736049、化合物2 回

生成物 1

HCID 90295830HCID 90295830、化合物収率 84.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide
溶媒

実験手順

Compound ((3R,3aS)-1-oxo-7-(3-oxomorpholin-4-yl)-1,3,3a,4-tetrahydrobenzo[b]oxazolo[3,4-d][1,4]oxazin-3-yl)methylmethanesulfonate (3.91 g, 9.81 mmol) prepared as above in (c) was dissolved in 50 ml of DMF. Phthalimide potassium (2.72 g, 14.72 mmol) was added and the mixture was allowed to react at 80° C. for 2 h. TLC (DCM/MeOH=10/1) was employed to monitor the reaction. After the reaction completed, water (80 ml) was added for dilution. There was white solid precipitated, which was filtered and dried. The filtrate was extracted with EA (50 ml×3). The organic phase was combined, and washed sequentially with water (30 ml) and saturated NaCl (30 ml) solution, dried over anhydrous sodium sulfate, filtered, and the solvent was evaporated to afford totally 3.71 g of white solid, yield: 84.2%.

後処理

  1. customto react at 80° C. for 2 h
  2. customthe reaction
  3. customprecipitated
  4. filtrationwhich was filtered
  5. customdried
  6. extractionThe filtrate was extracted with EA (50 ml×3)
  7. washwashed sequentially with water (30 ml) and saturated NaCl (30 ml) solution
  8. dry with materialdried over anhydrous sodium sulfate
  9. filtrationfiltered
  10. customthe solvent was evaporated

出典と根拠

ORDレコード
ord-17acac5298e64c52b92fedf69d40c0b4
出典データセット
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09382265B2

反応ノート

読み込み中…

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