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Diisopropylethylamine → HCID 86726715、化合物

HRID 1499481
ノート
印刷プレビュー

反応式

HRID 1499481 の反応式
Cl[C:2]1[C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[CH:6][N:5]=[C:4]2[N:13]([CH2:16][C:17]3[CH:22]=[CH:21][C:20]([O:23][CH3:24])=[CH:19][CH:18]=3)[N:14]=[CH:15][C:3]=12.[NH:25]1[CH2:30][CH2:29][CH2:28][C@H:27]([NH:31][C:32](=[O:38])[O:33][C:34]([CH3:37])([CH3:36])[CH3:35])[CH2:26]1.CCN(C(C)C)C(C)C>C(O)CCC>[C:34]([O:33][C:32]([NH:31][C@H:27]1[CH2:28][CH2:29][CH2:30][N:25]([C:2]2[C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[CH:6][N:5]=[C:4]3[N:13]([CH2:16][C:17]4[CH:22]=[CH:21][C:20]([O:23][CH3:24])=[CH:19][CH:18]=4)[N:14]=[CH:15][C:3]=23)[CH2:26]1)=[O:38])([CH3:37])([CH3:35])[CH3:36]
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

5

反応物 3

HCID 81531DiisopropylethylamineHCID 1514171tert-butyl N-[(3S)-piperidin-3-yl]carbamateHCID 53665897Ethyl 4-chloro-1-(4-methoxybenzyl)-1H-pyrazolo[3,4-b]pyridine-5-carboxylate

生成物 1

HCID 86726715HCID 86726715、化合物収率 86.7%

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

反応条件

温度
140 °C

実験手順

A mixture of ethyl 4-chloro-1-(4-methoxybenzyl)-1H-pyrazolo[3,4-b]pyridine-5-carboxylate (1.5 g, 4.3 mmol), tert-butyl (3S)-piperidin-3-ylcarbamate (1.0 g, 5.0 mmol) and DIPEA (0.84 g, 6.5 mmol) in 1-butanol (10 mL) was heated to 140° C. for 14 h, then allowed to cool. The mixture was concentrated under reduced pressure, and the resulting residue was diluted with EtOAc and washed with aq. NaHCO3. The organic extract was washed with water and brine, dried and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel using CombiFlash® apparatus, eluting with 20-100% EtOAc in hexanes, to give the sub-title compound (1.9 g, 86%). LCMS calc. for C27H36N5O5 (M+H)+: m/z=510.3. Found: 510.2.

後処理

  1. temperatureto cool
  2. concentrationThe mixture was concentrated under reduced pressure
  3. additionthe resulting residue was diluted with EtOAc
  4. washwashed with aq. NaHCO3
  5. extractionThe organic extract
  6. washwas washed with water and brine
  7. customdried
  8. concentrationconcentrated under reduced pressure
  9. customThe residue was purified by column chromatography on silica gel using CombiFlash® apparatus
  10. washeluting with 20-100% EtOAc in hexanes

出典と根拠

ORDレコード
ord-d6440e608d5f402f9e0181610cd447ee
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09200004B2

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