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 → 5-(3-(6-isopropoxypyridin-2-yl)-1H-indol-5-yl)-N-(piperidin-3-yl)-1,3,4-thiadiazol-2-amine

HRID 634177
ノート
印刷プレビュー

反応式

HRID 634177 の反応式
[CH:1]([O:4][C:5]1[N:10]=[C:9]([C:11]2[C:19]3[C:14](=[CH:15][CH:16]=[C:17]([C:20]4[S:24][C:23]([NH:25][CH:26]5[CH2:31][CH2:30][CH2:29][N:28](C(OC(C)(C)C)=O)[CH2:27]5)=[N:22][N:21]=4)[CH:18]=3)[N:13](S(C3C=CC(C)=CC=3)(=O)=O)[CH:12]=2)[CH:8]=[CH:7][CH:6]=1)([CH3:3])[CH3:2].Cl>O1CCOCC1.O.[OH-].[Na+]>[CH:1]([O:4][C:5]1[N:10]=[C:9]([C:11]2[C:19]3[C:14](=[CH:15][CH:16]=[C:17]([C:20]4[S:24][C:23]([NH:25][CH:26]5[CH2:31][CH2:30][CH2:29][NH:28][CH2:27]5)=[N:22][N:21]=4)[CH:18]=3)[NH:13][CH:12]=2)[CH:8]=[CH:7][CH:6]=1)([CH3:3])[CH3:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 313Hydrochloric AcidHCID 68328847tert-butyl 3-(5-(3-(6-isopropoxypyridin-2-yl)-1-tosyl-1H-indol-5-yl)-1,3,4-thiadiazol-2-ylamino)piperidine-1-carboxylate

生成物 1

HCID 683280335-(3-(6-isopropoxypyridin-2-yl)-1H-indol-5-yl)-N-(piperidin-3-yl)-1,3,4-thiadiazol-2-amine

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 14798Sodium Hydroxide
溶媒
3 回
HCID 312751,4-Dioxane溶媒

反応条件

温度
100 °C

実験手順

An orange solution of tert-butyl 3-(5-(3-(6-isopropoxypyridin-2-yl)-1-tosyl-1H-indol-5-yl)-1,3,4-thiadiazol-2-ylamino)piperidine-1-carboxylate (38.6 mg, 0.056 mmol) and aq. NaOH (2.0 M, 0.1 mL, 0.200 mmol) in dioxane (1.0 mL) was heated at 100° C. for 30 min. Additional aq. NaOH (2.0 M, 0.1 mL, 0.200 mmol) was added, and the resulting mixture was stirred at 100° C. for 1.5 h. The mixture was then concentrated in vacuo, and the residue was taken up in HCl (4.0 M in dioxane; 1.0 mL, 4.00 mmol). The resulting yellow-orange mixture was stirred at 25° C. for 1 h, diluted with H2O (4 mL) and 1 N aq NaOH (3.5 mL). The resulting mixture was partitioned between DCM (30 mL) and saturated aq NaHCO3 (20 mL). The organic layer was separated, and the aqueous layer was extracted with DCM (20 mL). The combined organic extracts were dried over sodium sulfate, filtered, and concentrated in vacuo to provide crude 5-(3-(6-isopropoxypyridin-2-yl)-1H-indol-5-yl)-N-(piperidin-3-yl)-1,3,4-thiadiazol-2-amine as a light-yellow solid, which was taken up in DMSO (2.0 mL) and purified by reverse phase HPLC (10-100% AcCN/H2O+0.1% TFA) to provide 5-(3-(6-isopropoxypyridin-2-yl)-1H-indol-5-yl)-N-(piperidin-3-yl)-1,3,4-thiadiazol-2-amine 2,2,2-trifluoroacetate (12.0 mg, 0.022 mmol, 39%) as a yellow oil: MS (ESI, pos. ion) m/z: 435.2 (M+1). 1H NMR (400 MHz, MeOH-d4) δ ppm 11.38 (br s, 1H), 8.80 (d, J=1.2 Hz, 1H), 7.98 (s, 1H), 7.75-7.79 (m, 1H), 7.71-7.75 (m, 1H), 7.54 (d, J=8.6 Hz, 1H), 7.43 (d, J=7.4 Hz, 1H), 6.66 (d, J=8.2 Hz, 1H), 5.53 (dt, J=12.2, 6.1 Hz, 1H), 4.07-4.16 (m, 1H), 3.68 (dd, J=12.2, 3.6 Hz, 1H), 3.34-3.35 (obsc m, 1H), 3.09-3.15 (m, 1H), 3.02-3.08 (m, 1H), 2.18-2.27 (m, 1H), 2.10 (dt, J=15.0, 5.1 Hz, 1H), 1.83-1.92 (m, 1H), 1.73-1.82 (m, 1H), 1.49-1.51 (m, 3H), 1.49 (s, 3H).

後処理

  1. concentrationThe mixture was then concentrated in vacuo
  2. stirringThe resulting yellow-orange mixture was stirred at 25° C. for 1 h
  3. customThe resulting mixture was partitioned between DCM (30 mL) and saturated aq NaHCO3 (20 mL)
  4. customThe organic layer was separated
  5. extractionthe aqueous layer was extracted with DCM (20 mL)
  6. dry with materialThe combined organic extracts were dried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-3a83984372444b3fb97a054c2c3dd72d
出典データセット
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09321756B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート