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

Hydrochloric Acid → 4-(4',5'-difluoro-2'-methoxy-biphenyl-4-yloxymethyl)-1H-indazole

HRID 551494
ノート
印刷プレビュー

反応式

HRID 551494 の反応式
[F:1][C:2]1[C:7]([F:8])=[CH:6][C:5]([C:9]2[CH:14]=[CH:13][C:12]([O:15][CH2:16][C:17]3[CH:25]=[CH:24][CH:23]=[C:22]4[C:18]=3[CH:19]=[N:20][N:21]4C3CCCCO3)=[CH:11][CH:10]=2)=[C:4]([O:32][CH3:33])[CH:3]=1.Cl.CCOC(C)=O.O>CO>[F:1][C:2]1[C:7]([F:8])=[CH:6][C:5]([C:9]2[CH:10]=[CH:11][C:12]([O:15][CH2:16][C:17]3[CH:25]=[CH:24][CH:23]=[C:22]4[C:18]=3[CH:19]=[N:20][NH:21]4)=[CH:13][CH:14]=2)=[C:4]([O:32][CH3:33])[CH: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 313Hydrochloric AcidHCID 962Water2 回HCID 8857Ethyl AcetateHCID 671519344-(4',5'-difluoro-2'-methoxy-biphenyl-4-yloxymethyl)-1-(tetrahydro-pyran-2-yl)-1H-indazole

生成物 1

HCID 529396104-(4',5'-difluoro-2'-methoxy-biphenyl-4-yloxymethyl)-1H-indazole収率 73.8%

試薬・触媒・溶媒 1

HCID 887
Methanol
溶媒

実験手順

4-(4′,5′-Difluoro-2′-methoxy-biphenyl-4-yloxymethyl)-1-(tetrahydro-pyran-2-yl)-1H-indazole (0.4 g, 0.888 mmol) and 1N HCl (1.8 mL, 1.8 mmol) in 10 mL MeOH were heated to reflux for 5 hrs. The reaction was cooled and distributed between EtOAc and H2O. The water layer was made basic to pH 12 and the organic layer was separated and concentrated in vacuo. The crude product was purified by flash chromatography with a gradient from 20-100% ethyl acetate in hexanes to yield 4-(4′,5′-difluoro-2′-methoxy-biphenyl-4-yloxymethyl)-1H-indazole as a white solid (240 mg, 73.7%). LC-MS (ES) calculated for C21H16F2N2O2, 366.37; found m/z 367 [M+H]+.

後処理

  1. temperatureto reflux for 5 hrs
  2. temperatureThe reaction was cooled
  3. customthe organic layer was separated
  4. concentrationconcentrated in vacuo
  5. customThe crude product was purified by flash chromatography with a gradient from 20-100% ethyl acetate in hexanes

出典と根拠

ORDレコード
ord-d0c4d16b7b714b01a2446624cfa91ac6
出典データセット
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07947728B1

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