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

Sodium Bicarbonate → HCID 70874808、化合物

HRID 2172270
ノート
印刷プレビュー

反応式

HRID 2172270 の反応式
[F:1][C:2]([F:12])([F:11])[O:3][C:4]1[CH:10]=[CH:9][C:7]([NH2:8])=[CH:6][CH:5]=1.[N+:13]([C:16]1[N:17]=[C:18]2[N:23]([CH:24]=1)[CH2:22][CH2:21][C@H:20]([CH2:25][O:26][C:27]1[CH:32]=[CH:31][C:30]([N:33]3[CH2:38][CH2:37][C:36](=O)[CH2:35][CH2:34]3)=[CH:29][CH:28]=1)[O:19]2)([O-:15])=[O:14].C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(=O)([O-])O.[Na+]>C(O)(=O)C.ClCCCl>[N+:13]([C:16]1[N:17]=[C:18]2[N:23]([CH:24]=1)[CH2:22][CH2:21][C@H:20]([CH2:25][O:26][C:27]1[CH:32]=[CH:31][C:30]([N:33]3[CH2:38][CH2:37][CH:36]([NH:8][C:7]4[CH:9]=[CH:10][C:4]([O:3][C:2]([F:11])([F:12])[F:1])=[CH:5][CH:6]=4)[CH2:35][CH2:34]3)=[CH:29][CH:28]=1)[O:19]2)([O-:15])=[O:14]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 516892Sodium BicarbonateHCID 6008484-(Trifluoromethoxy)anilineHCID 5049666Sodium triacetoxyborohydrideHCID 70874615HCID 70874615、化合物

生成物 1

HCID 70874808HCID 70874808、化合物

試薬・触媒・溶媒 2

HCID 111,2-Dichloroethane溶媒
HCID 176Acetic Acid溶媒

実験手順

4-(Trifluoromethoxy)aniline (1.271 ml) was added to a 1,2-dichloroethane solution (50 ml) of 1-[4-((R)-2-nitro-6,7-dihydro-5H-imidazo[2,1-b][1,3]oxazin-7-ylmethoxy)phenyl]piperidin-4-one (2.5 g). Subsequently, sodium triacetoxyborohydride (1.992 g) and acetic acid (0.538 ml) were added thereto and the mixture was stirred at room temperature for 21 hours. A saturated sodium hydrogen carbonate aqueous solution was added to the reaction mixture, followed by extraction with methylene chloride. The organic layer was washed with a saturated sodium chloride aqueous solution and dried over anhydrous sodium sulfate. Thereafter, the solvent was distilled off under reduced pressure. The resulting residue was purified by silica gel column chromatography (ethyl acetate:n-hexane=1:1) and recrystallized from ethyl acetate to afford the title compound as a yellow powder (2.55 g).

後処理

  1. extractionfollowed by extraction with methylene chloride
  2. washThe organic layer was washed with a saturated sodium chloride aqueous solution
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationThereafter, the solvent was distilled off under reduced pressure
  5. customThe resulting residue was purified by silica gel column chromatography (ethyl acetate:n-hexane=1:1)
  6. customrecrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-19a9bb5aaf0a48089107a58fa2c7006c
出典データセット
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09051333B2

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