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1-Iodonaphthalene → 4-chloro-6-(1-naphthyl)-7-(phenylsulfonyl)-7H-pyrrolo[2,3-d]pyrimidine

HRID 1747677
ノート
印刷プレビュー

反応式

HRID 1747677 の反応式
C(NC(C)C)(C)C.C([Li])CCC.[Cl:13][C:14]1[C:15]2[CH:22]=[CH:21][N:20]([S:23]([C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=3)(=[O:25])=[O:24])[C:16]=2[N:17]=[CH:18][N:19]=1.I[C:33]1[C:42]2[C:37](=[CH:38][CH:39]=[CH:40][CH:41]=2)[CH:36]=[CH:35][CH:34]=1>C1COCC1.CCCCCC.[Cl-].[Zn+2].[Cl-].C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[Cl:13][C:14]1[C:15]2[CH:22]=[C:21]([C:41]3[C:42]4[C:37](=[CH:36][CH:35]=[CH:34][CH:33]=4)[CH:38]=[CH:39][CH:40]=3)[N:20]([S:23]([C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=3)(=[O:25])=[O:24])[C:16]=2[N:17]=[CH:18][N:19]=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

9

反応物 4

HCID 70041-IodonaphthaleneHCID 7912DiisopropylamineHCID 109463064-Chloro-7-(phenylsulfonyl)-7H-pyrrolo[2,3-D]pyrimidineHCID 178418339Butyllithium

生成物 1

HCID 866187344-chloro-6-(1-naphthyl)-7-(phenylsulfonyl)-7H-pyrrolo[2,3-d]pyrimidine収率 93.2%

試薬・触媒・溶媒 4

HCID 3007855
Zincchloride
触媒
HCID 178418397HCID 178418397、化合物触媒
HCID 8028Tetrahydrofuran溶媒4 回
HCID 8058Hexane溶媒

反応条件

温度
-78 °C

実験手順

To a stirred solution of N,N-diisopropylamine (265 μL, 1.89 mmol) in THF (3.00 mL) was added dropwise 1.60 M n-butyllithium in hexane (1.17 mL) at −78° C. under an atmosphere of Argon, and the mixture was stirred for 20 minutes at −78° C. To this mixture was added dropwise a solution of 4-chloro-7-(phenylsulfonyl)-7H-pyrrolo[2,3-d]pyrimidine (500 mg, 1.70 mmol) in THF (5.00 mL), and the mixture was stirred for 1 h at −78° C. A solution of zinc chloride (278 mg, 2.04 mmol) in THF (2.00 mL) was added dropwise, and the resulting mixture was taken out the cooling bath and allowed to stir for 1 h. To a suspension of tetrakis(triphenylphosphine)palladium(0) (100 mg, 0.08 mmol) in THF (2.00 mL) was added 1-iodonaphthalene (0.30 mL, 2.06 mmol), and the resulting yellow solution was immediately added to the reaction mixture. The resulting mixture was heated at 80° C. for 1 h. After cooling to 23° C., the reaction mixture was quenched by the addition of water (70.0 mL) and the water layer was acidified with 1.00 M hydrochloric acid. The mixture was extracted with DCM (3×100 mL), and the organic layers were combined. The organic layer was washed with brine, dried over MgSO4, filtered, and evaporated under vacuum. The residue was purified via silica gel column chromatography eluting with 30% ethyl acetate in hexanes to afford the title compound (665 mg, 82%). LC/MS: Rt=11.11 min, ES+ 420.0 (FA long).

後処理

  1. stirringthe mixture was stirred for 1 h at −78° C
  2. stirringto stir for 1 h
  3. additionthe resulting yellow solution was immediately added to the reaction mixture
  4. temperatureThe resulting mixture was heated at 80° C. for 1 h
  5. temperatureAfter cooling to 23° C.
  6. customthe reaction mixture was quenched by the addition of water (70.0 mL)
  7. extractionThe mixture was extracted with DCM (3×100 mL)
  8. washThe organic layer was washed with brine
  9. dry with materialdried over MgSO4
  10. filtrationfiltered
  11. customevaporated under vacuum
  12. customThe residue was purified via silica gel column chromatography
  13. washeluting with 30% ethyl acetate in hexanes

出典と根拠

ORDレコード
ord-944a949fb63a441f8c122b8eb5c3c6fa
出典データセット
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09150525B2

反応ノート

読み込み中…

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