Lithium Hexamethyldisilazide → 4-(4-(3,3-Diphenyl-2-propenyl)-1-piperazinyl)benzenecarboximidamide

HRID 731545

反応式

HRID 731545 の反応式
[C:1]1([C:7]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)=[CH:8][CH2:9][N:10]2[CH2:15][CH2:14][N:13]([C:16]3[CH:23]=[CH:22][C:19]([C:20]#[N:21])=[CH:18][CH:17]=3)[CH2:12][CH2:11]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Li+].C[Si]([N-:35][Si](C)(C)C)(C)C>O1CCCC1>[C:24]1([C:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)=[CH:8][CH2:9][N:10]2[CH2:11][CH2:12][N:13]([C:16]3[CH:17]=[CH:18][C:19]([C:20](=[NH:35])[NH2:21])=[CH:22][CH:23]=3)[CH2:14][CH2:15]2)[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1

参加物

4

反応物 2

HCID 2733832Lithium HexamethyldisilazideHCID 591866114-(4-(3,3-Diphenyl-2-propenyl)-1-piperazinyl)benzonitrile

生成物 1

HCID 591866074-(4-(3,3-Diphenyl-2-propenyl)-1-piperazinyl)benzenecarboximidamide収率 83.4%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of EXAMPLE 12A (0.515 g, 1.36 mmol) in dry tetrahydrofuran (6 mL) was treated dropwise with LiHMDS (1M, 6.8 mL, 6.8 mmol), stirred for 16 hours, quenched with 1N HCl (8 mL), and filtered. The filter cake was collected to provide the desired product (0.45 g, 71%) that was used without further purification. MS (CI) m/e 397 (M+H)+.

後処理

  1. customquenched with 1N HCl (8 mL)
  2. filtrationfiltered
  3. customThe filter cake was collected

出典と根拠

ORDレコード
ord-f615de3334bf4e5d8dc073a1350c2764
出典データセット
uspto-grants-2009_09
特許番号
US07585858B2

関連ノート

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