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

Triethylamine → HCID 18396233、化合物

HRID 611589
ノート
印刷プレビュー

反応式

HRID 611589 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4](I)[C:3]=1[OH:9].CCN(CC)CC.[C:17]([N:24]1[CH2:28][CH2:27][CH2:26][C@H:25]1[C:29]#[CH:30])([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18].C([O-])(O)=O.[Na+]>CN(C=O)C.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.[Cu]I>[C:17]([N:24]1[CH2:28][CH2:27][CH2:26][C@H:25]1[C:29]1[O:9][C:3]2[C:4](=[N:5][CH:6]=[CH:7][C:2]=2[Cl:1])[CH:30]=1)([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 8471TriethylamineHCID 516892Sodium BicarbonateHCID 11030701(S)-N-Boc-2-ethynylpyrrolidineHCID 195976654-Chloro-2-iodopyridin-3-ol

生成物 1

HCID 18396233HCID 18396233、化合物収率 14%

試薬・触媒・溶媒 3

HCID 24350
Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)
触媒
HCID 178418476HCID 178418476、化合物触媒
HCID 6228Dimethylformamide溶媒2 回

実験手順

To a solution of 4-chloro-3-hydroxy-2-iodopyridine (1.04 g, 4.10 mmol) in DMF (10 mL) was added (Ph3P)2PdCl2 (0.140 g, 0.20 mmol), CuI (0.152 g, 0.80 mmol) and Et3N (0.496 g, 4.90 mmol). The mixture was stirred at room temperature for one hour. A solution of 1-Boc-2-(S)-ethynylpyrrolidine (0.80 g, 4.10 mmol), from step 1c above, in DMF (10 mL) was added and the mixture was heated at 60° C. for 16 hours. The reaction mixture was cooled to room temperature and poured into saturated NaHCO3 and washed with Et2O (4×100 mL). The combined organic extracts were washed with brine/H2O (1/1 400 mL), dried (MgSO4), and concentrated. The crude product was chromatographed (silica gel; CH2Cl2 /MeOH, 90:10) to afford the title compound as a brown oil (0.180 g, 14%): 1H NMR (CDCl3, 300 MHz) δ 1.40 (s, 9H), 1.95-2.10 (m, 4H), 3.10-3.25 (m, 2H), 4.90-5.10 (m, 1H), 6.65 (s, 1H), 7.10 (br s, 1H), 8.38 (br s, 1H); MS (DCI/NH3) m/z: 323 (M+H)+.

後処理

  1. temperaturethe mixture was heated at 60° C. for 16 hours
  2. temperatureThe reaction mixture was cooled to room temperature
  3. washwashed with Et2O (4×100 mL)
  4. washThe combined organic extracts were washed with brine/H2O (1/1 400 mL)
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated
  7. customThe crude product was chromatographed (silica gel; CH2Cl2 /MeOH, 90:10)

出典と根拠

ORDレコード
ord-a0618f21e0e540c8812d0b7f44ffd79c
出典データセット
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06001849

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