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

2-Bromo-m-xylene → (1-(2,6-Dimethylphenyl)pyrrolidin-3-yl)methanol

HRID 469161
ノート
印刷プレビュー

反応式

HRID 469161 の反応式
Br[C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[CH:4][C:3]=1[CH3:9].Cl.[NH:11]1[CH2:15][CH2:14][CH:13]([CH2:16][OH:17])[CH2:12]1.C1(P(C2CCCCC2)C2C=CC=CC=2C2C(OC)=CC=CC=2OC)CCCCC1.C[Si](C)(C)[N-][Si](C)(C)C.[Li+].O.C(=O)(O)[O-].[Na+]>O1CCCC1.[Pd].C(=CC(C=CC1C=CC=CC=1)=O)C1C=CC=CC=1.C(=CC(C=CC1C=CC=CC=1)=O)C1C=CC=CC=1.C(OCC)(=O)C>[CH3:9][C:3]1[CH:4]=[CH:5][CH:6]=[C:7]([CH3:8])[C:2]=1[N:11]1[CH2:15][CH2:14][CH:13]([CH2:16][OH:17])[CH2:12]1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 684712-Bromo-m-xyleneHCID 2733832Lithium hexamethyldisilazaneHCID 112698722-Dicyclohexylphosphino-2',6'-dimethoxybiphenylHCID 23080030(Pyrrolidin-3-yl)methanol hydrochlorideHCID 86585896Sodium bicarbonate water

生成物 1

HCID 24275467(1-(2,6-Dimethylphenyl)pyrrolidin-3-yl)methanol
収率 27.8%

試薬・触媒・溶媒 3

HCID 1542701,5-Diphenylpenta-1,4-dien-3-one;palladium触媒HCID 8028Tetrahydrofuran溶媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 2-bromo-1,3-dimethylbenzene (500 mg), pyrrolidine-3-yl methanol hydrochloride (409 mg), bis(dibenzylideneacetone) palladium (155 mg), and 2-dicyclohexylphosphino-2′,6′-dimethoxybiphenyl (SPhos; 222 mg) in tetrahydrofuran (5 mL), molecular sieves 4A (powder; 410 mg) were added. To the mixed solution, a solution (8.9 mL) of 1.0 M lithium hexamethyldisilazide in tetrahydrofuran was added, and the resultant reaction mixture was heated and refluxed for 2.5 hours. To the reaction solution, saturated sodium bicarbonate water and ethyl acetate were added, and the resultant reaction mixture was extracted with ethyl acetate. The organic phase was washed with a saturated saline and was dried over anhydrous sodium sulfate. From the organic phase, the solvent was distilled off under reduced pressure, followed by purifying the resultant residue by silica gel column chromatography (eluate; n-hexane:ethyl acetate=100:0 to 75:25), and from the resultant, the solvent was distilled off under reduced pressure to obtain the subject compound (154 mg) as a yellow oily substance.

後処理

  1. customthe resultant reaction mixture
  2. temperaturewas heated
  3. temperaturerefluxed for 2.5 hours
  4. customthe resultant reaction mixture
  5. extractionwas extracted with ethyl acetate
  6. washThe organic phase was washed with a saturated saline
  7. dry with materialwas dried over anhydrous sodium sulfate
  8. distillationFrom the organic phase, the solvent was distilled off under reduced pressure
  9. customby purifying the resultant residue by silica gel column chromatography (eluate; n-hexane:ethyl acetate=100:0 to 75:25)
  10. distillationfrom the resultant, the solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-485d3bb5f2b940ad80c6864ebee202d9
出典データセット
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08629102B2

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