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 hydride → HCID 44540141、化合物

HRID 1616051
ノート
印刷プレビュー

反応式

HRID 1616051 の反応式
[H-].[Na+].[O:3]1[CH2:8][CH2:7][CH:6]([OH:9])[CH2:5][CH2:4]1.[H][H].F[C:13]1[N:18]=[C:17]([C:19]([NH:21][C:22]2[CH:30]=[C:29]([C:31]3[CH:39]=[CH:38][CH:37]=[C:36]4[C:32]=3[CH:33]=[CH:34][NH:35]4)[CH:28]=[C:27]3[C:23]=2[CH:24]=[N:25][NH:26]3)=[O:20])[CH:16]=[CH:15][CH:14]=1>C1COCC1.O>[NH:35]1[C:36]2[C:32](=[C:31]([C:29]3[CH:28]=[C:27]4[C:23]([CH:24]=[N:25][NH:26]4)=[C:22]([NH:21][C:19]([C:17]4[CH:16]=[CH:15][CH:14]=[C:13]([O:9][CH:6]5[CH2:7][CH2:8][O:3][CH2:4][CH2:5]5)[N:18]=4)=[O:20])[CH:30]=3)[CH:39]=[CH:38][CH:37]=2)[CH:33]=[CH:34]1
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 24758Sodium hydride2 回HCID 74956Tetrahydro-4H-pyran-4-ol2 回HCID 44541051HCID 44541051、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 44540141HCID 44540141、化合物収率 11%

試薬・触媒・溶媒 2

HCID 962Water
溶媒
HCID 8028Tetrahydrofuran溶媒

実験手順

Under an atmosphere of nitrogen, sodium hydride (5 mg, 0.14 mmol, 60% suspension in mineral oil) was added to a solution of tetrahydro-2H-pyran-4-ol (13 mg, 0.14 mmol) in THF (2 ml). After hydrogen evolution was complete, 6-Fluoro-N-[6-(1H-indol-4-yl)-1H-indazol-4-yl]-2-pyridinecarboxamide (50 mg, 0.14 mmol) was added and the mixture was heated to reflux for 1 h. Another portion of tetrahydro-2H-pyran-4-ol (13 mg, 0.14 mmol) and sodium hydride (5 mg, 0.14 mmol) was added and the mixture was heated to reflux overnight. The mixture was cooled to room temperature, water was added and the mixture was extracted with DCM. The organic extracts were combined, dried over MgSO4, filtered and the solvent was removed in vacuo to give an orange oil. This was purified by mass-directed automated preparative HPLC (Method B) to give the title compound (7 mg) as a white solid.

後処理

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 1 h
  3. temperaturethe mixture was heated
  4. temperatureto reflux overnight
  5. extractionthe mixture was extracted with DCM
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. customthe solvent was removed in vacuo
  9. customto give an orange oil
  10. customThis was purified

出典と根拠

ORDレコード
ord-ca28dd38900342f3a79a24fa9dc28ecb
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08765743B2

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