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

Diisopropylethylamine → HCID 70817143、化合物

HRID 82125
ノート
印刷プレビュー

反応式

HRID 82125 の反応式
Cl.[N:2]1[C:11]2[CH2:10][N:9]([CH2:12][C:13]([OH:15])=O)[CH2:8][CH2:7][C:6]=2[CH:5]=[CH:4][CH:3]=1.[NH2:16][C:17]1[CH:18]=[C:19]([C:23]([C:25]2[C:33]3[CH:32]=[N:31][CH:30]=[N:29][C:28]=3[N:27]([CH:34]([CH3:36])[CH3:35])[CH:26]=2)=[O:24])[CH:20]=[N:21][CH:22]=1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(C(C)C)C(C)C>C(OCC)(=O)C.CN(C=O)C>[N:2]1[C:11]2[CH2:10][N:9]([CH2:12][C:13]([NH:16][C:17]3[CH:22]=[N:21][CH:20]=[C:19]([C:23]([C:25]4[C:33]5[CH:32]=[N:31][CH:30]=[N:29][C:28]=5[N:27]([CH:34]([CH3:36])[CH3:35])[CH:26]=4)=[O:24])[CH:18]=3)=[O:15])[CH2:8][CH2:7][C:6]=2[CH:5]=[CH:4][CH:3]=1
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

7

反応物 4

HCID 81531DiisopropylethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 70817456(5-aminopyridin-3-yl)(7-isopropyl-7H-pyrrolo[2,3-d]pyrimidin-5-yl)methanoneHCID 70817716(5,8-Dihydro-6H-[1,7]naphthyridin-7-yl)-acetic acid hydrochloride

生成物 1

HCID 70817143HCID 70817143、化合物
収率 26%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
50 °C

実験手順

To a DMF solution of (5,8-Dihydro-6H-[1,7]naphthyridin-7-yl)-acetic acid hydrochloride (Preparation 235) (34.2 mg, 0.18 mmol) were added (5-Amino-pyridin-3-yl)-(7-isopropyl-7H-pyrrolo[2,3-d]pyrimidin-5-yl)-methanone (Preparation 95) (50 mg, 0.18 mmol), HATU (136.4 mg, 0.36 mmol) and Hunig's base (0.092 ml, 0.54 mmol). The mixture was heated at 50° C. for 20 hours and then diluted with ethyl acetate, washed with water, brine, dried over sodium sulphate and evaporated to dryness in vacuo. The crude solid was purified over preparative TLC eluting with 5% MeOH/EtOAc to afford the title compound as off white solid in 26% yield, 21 mg. 1H NMR (400 MHz, DMSO-D6) δ: 1.55 (d, 6H), 2.85-2.92 (m, 4H), 3.45 (s, 2H), 3.80 (s, 2H), 5.10 (m, 1H), 7.19 (dd, 1H), 7.56 (d, 1H), 8.32 (d, 1H), 8.53 (s, 1H), 8.56 (t, 1H), 8.73 (d, 1H), 8.99 (s, 1H), 9.07 (d, 1H), 9.45 (s, 1H), 10.31 (s, 1H); LCMS (system 9): Rt=1.77 min; m/z 456 [M+H]+.

後処理

  1. washwashed with water, brine
  2. dry with materialdried over sodium sulphate
  3. customevaporated to dryness in vacuo
  4. customThe crude solid was purified over preparative TLC
  5. washeluting with 5% MeOH/EtOAc

出典と根拠

ORDレコード
ord-46a158f66223483983842b65f408510a
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08846698B2

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