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

Lithium Hydroxide → HCID 59671517、化合物

HRID 549766
ノート
印刷プレビュー

反応式

HRID 549766 の反応式
[OH-].[Li+].[C:3]([O:7][C:8]([N:10]1[CH2:15][CH2:14][N:13]([C:16]2[O:17][C:18]([C:22]([O:24]CC)=O)=[C:19]([CH3:21])[N:20]=2)[CH:12]([CH2:27][O:28][C:29]2[CH:30]=[N:31][CH:32]=[CH:33][CH:34]=2)[CH2:11]1)=[O:9])([CH3:6])([CH3:5])[CH3:4].[CH2:35]([NH2:42])[C:36]1[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=1.C(N(CC)CC)C.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F>C1COCC1.CO.O>[CH2:35]([NH:42][C:22]([C:18]1[O:17][C:16]([N:13]2[CH2:14][CH2:15][N:10]([C:8]([O:7][C:3]([CH3:5])([CH3:4])[CH3:6])=[O:9])[CH2:11][CH:12]2[CH2:27][O:28][C:29]2[CH:30]=[N:31][CH:32]=[CH:33][CH:34]=2)=[N:20][C:19]=1[CH3:21])=[O:24])[C:36]1[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 3939Lithium HydroxideHCID 7504BenzylamineHCID 8471TriethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 59671499Ethyl 2-(4-(tert-butoxycarbonyl)-2-((pyridin-3-yloxy)methyl)piperazin-1-yl)-4-methyloxazole-5-carboxylate

生成物 1

HCID 59671517
HCID 59671517、化合物

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Lithium hydroxide (56 mg, 1.3 mmol) was added to a solution of ethyl 2-(4-(tert-butoxycarbonyl)-2-((pyridin-3-yloxy)methyl)piperazin-1-yl)-4-methyloxazole-5-carboxylate (200 mg, 0.448 mmol) in THF (2 mL), MeOH (2 mL), and water (1 mL). After 3 h, 2.5 mL of the reaction mixture was removed and acidified to pH ˜3 with 1 N aqueous HCl. This was diluted with water (15 mL) and extracted with EtOAc (3×30 mL). The combined extracts were dried over Na2SO4, filtered, and concentrated under reduced pressure. The resulting yellow oil was dissolved in DMF (3 mL) and benzylamine (0.027 mL, 0.246 mmol), triethylamine (0.094 mL, 0.672 mmol) and TBTU (108 mg, 0.336 mmol) were added. After 14 h, the reaction mixture was concentrated under reduced pressure and purified by HPLC (5 to 95% MeCN/0.1% TFA in H2O/0.1% TFA gradient). This gave the title compound as a brown solid. LC-MS: RT=7.79 min, [M+H]+=508.9.

後処理

  1. custom2.5 mL of the reaction mixture was removed
  2. additionThis was diluted with water (15 mL)
  3. extractionextracted with EtOAc (3×30 mL)
  4. dry with materialThe combined extracts were dried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. dissolutionThe resulting yellow oil was dissolved in DMF (3 mL)
  8. waitAfter 14 h
  9. concentrationthe reaction mixture was concentrated under reduced pressure
  10. custompurified by HPLC (5 to 95% MeCN/0.1% TFA in H2O/0.1% TFA gradient)

出典と根拠

ORDレコード
ord-3fa03e2414dc49dcaa589d3f4857c07b
出典データセット
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07943622B2

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