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3,5-Dibromopyridine → (3aR,6aS)-tert-butyl 5-(5-bromopyridin-3-yl)hexahydropyrrolo[3,4-c]pyrrole-2(1H)-carboxylate

HRID 240533
ノート
印刷プレビュー

反応式

HRID 240533 の反応式
[CH2:1]1[C@@H:5]2[CH2:6][NH:7][CH2:8][C@@H:4]2[CH2:3][N:2]1[C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10].[Br:16][C:17]1[CH:18]=[N:19][CH:20]=[C:21](Br)[CH:22]=1.CC(C)([O-])C.[Na+]>C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].C1(C)C=CC=CC=1>[Br:16][C:17]1[CH:22]=[C:21]([N:7]2[CH2:6][C@@H:5]3[CH2:1][N:2]([C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:3][C@@H:4]3[CH2:8]2)[CH:20]=[N:19][CH:18]=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

6

反応物 3

HCID 693693,5-DibromopyridineHCID 1514452Cis-2-boc-hexahydropyrrolo[3,4-C]pyrroleHCID 23676156Sodium t-butoxide

生成物 1

HCID 44189936(3aR,6aS)-tert-butyl 5-(5-bromopyridin-3-yl)hexahydropyrrolo[3,4-c]pyrrole-2(1H)-carboxylate収率 54.3%

試薬・触媒・溶媒 2

HCID 9811564Bis(dibenzylideneacetone)palladium
触媒
HCID 1140Toluene溶媒2 回

反応条件

温度
70 °C

実験手順

The product from example 1C (541 mg, 2.55 mmol) and 3,5-dibromopyridine (724 mg, 3.06 mmol) were combined in a 100 mL flask with toluene (14 mL). The solution was stirred at room temperature as sodium t-butoxide (367 mg, 3.82 mmol) was added as a solid. In a test tube, racemic-2,2′-bis(diphenylphosphino-1,1′-binaphthyl) (31 mg, 0.05 mmol) and tris(dibenzylideneacetone)dipalladium (0) (22 mg, 0.024 mmol) were combined with toluene (2 mL) and the mixture was heated at 70° C. for 5 min, then cooled to room temperature. This mixture was rinsed into the 100 mL flask with toluene (2 mL), and the reaction flask was evacuated and purged with nitrogen (3 cycles). The mixture was heated at 80° C. for 20 h, then cooled to room temperature and loaded onto a column of silica gel (45 g) and eluted with hexanes-EtOAc (1:1) to provide the titled compound as an off-white solid (0.51 g, 54%). 1H NMR (300 MHz, CD3OD) δ ppm 1.45 (s, 9H), 3.00-3.14 (m, 2H), 3.20-3.28 (m, 2H), 3.26-3.31 (m, 2H), 3.50-3.59 (m, 2H), 3.59-3.71 (m, 2H), 7.14-7.19 (m, 1H), 7.79-7.90 (m, 2H).

後処理

  1. additionwas added as a solid
  2. temperaturecooled to room temperature
  3. washThis mixture was rinsed into the 100 mL flask with toluene (2 mL)
  4. customthe reaction flask was evacuated
  5. custompurged with nitrogen (3 cycles)
  6. temperatureThe mixture was heated at 80° C. for 20 h
  7. temperaturecooled to room temperature
  8. washeluted with hexanes-EtOAc (1:1)

出典と根拠

ORDレコード
ord-9ad80728c8a04ed89daed63b698cf700
出典データセット
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08648084B2

反応ノート

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