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Ammonium Chloride → 2-(1-Pyridin-2-yl-cyclopentyl)-acetamidine hydrochloride

HRID 2169465
ノート
印刷プレビュー

反応式

HRID 2169465 の反応式
[NH4+:1].[Cl-:2].C[Al](C)C.[N:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[C:13]1([CH2:18][C:19]#[N:20])[CH2:17][CH2:16][CH2:15][CH2:14]1>C1(C)C=CC=CC=1>[ClH:2].[N:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[C:13]1([CH2:18][C:19]([NH2:1])=[NH:20])[CH2:17][CH2:16][CH2:15][CH2:14]1
参加物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 25517Ammonium ChlorideHCID 16682925TrimethylaluminumHCID 86726092(1-Pyridin-2-yl-cyclopentyl)-acetonitrile

生成物 1

HCID 867260932-(1-Pyridin-2-yl-cyclopentyl)-acetamidine hydrochloride収率 80%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

To a stirred suspension of NH4Cl (1.05 g, 19.355 mmol) in dry toluene (15 mL) was added tri-methyl aluminum (2M) (5.2 mL, 10.323 mmol) at 5° C. The reaction mixture was warmed to room temperature and the reaction mixture was stirred for 2 h. A solution of (1-pyridin-2-yl-cyclopentyl)-acetonitrile (434) (1.2 g, 6.45 mmol) in toluene (5 mL) was added to above reaction mixture and the reaction mixture was stirred for 14 h at 100° C. After completion of the reaction, the reaction mixture was quenched with a suspension of silica gel (5 g) in chloroform (30 mL) and reaction mixture was stirred for half an hour at room temperature. It was filtered through a sintered funnel and the residue (silica gel) was washed with methanol (30 mL). The combined filtrate was concentrated and the resulting crude mass was stirred with 10% methanol in dichloromethane (100 mL). The thus generated suspension was filtered and the filtrate was concentrated under reduced pressure to get 2-(1-pyridin-2-yl-cyclopentyl)-acetamidine hydrochloride (435) (1.05 g, 80%) as a white solid.

後処理

  1. stirringthe reaction mixture was stirred for 14 h at 100° C
  2. customAfter completion of the reaction
  3. customthe reaction mixture was quenched with a suspension of silica gel (5 g) in chloroform (30 mL) and reaction mixture
  4. stirringwas stirred for half an hour at room temperature
  5. filtrationIt was filtered through a sintered funnel
  6. washthe residue (silica gel) was washed with methanol (30 mL)
  7. concentrationThe combined filtrate was concentrated
  8. stirringthe resulting crude mass was stirred with 10% methanol in dichloromethane (100 mL)
  9. filtrationThe thus generated suspension was filtered
  10. concentrationthe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-40551ae1b50948f486acfbc8aeba5066
出典データセット
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09045486B2

反応ノート

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