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HCID 86630875、化合物 → 4,5-Diamino-6-[(3S)-3-(dimethylamino)pyrrolidin-1-yl]-2-methylbiphenyl-3-carbonitrile

HRID 17554
ノート
印刷プレビュー

反応式

HRID 17554 の反応式
[NH2:1][C:2]1[C:7]([N+:8]([O-])=O)=[C:6]([N:11]2[CH2:15][CH2:14][C@H:13]([N:16]([CH3:18])[CH3:17])[CH2:12]2)[C:5]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[C:4]([CH3:25])[C:3]=1[C:26]#[N:27]>O.O.O.O.O.O.[Fe](Cl)Cl.[Zn].CN(C)C=O>[NH2:1][C:2]1[C:7]([NH2:8])=[C:6]([N:11]2[CH2:15][CH2:14][C@H:13]([N:16]([CH3:17])[CH3:18])[CH2:12]2)[C:5]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[C:4]([CH3:25])[C:3]=1[C:26]#[N:27]
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 1

HCID 86630875HCID 86630875、化合物

生成物 1

HCID 866308764,5-Diamino-6-[(3S)-3-(dimethylamino)pyrrolidin-1-yl]-2-methylbiphenyl-3-carbonitrile収率 97.3%

試薬・触媒・溶媒 3

HCID 23994Zinc触媒HCID 129819097HCID 129819097、化合物触媒HCID 6228Dimethylformamide溶媒

実験手順

An aqueous solution (14 ml) of iron chloride hexahydrate (0.83 g, 3.06 mmol) and zinc (5.01 g, 76.6 mmol) were added to an N,N-dimethylformamide (35 ml) solution of 4-amino-6-[(3S)-3-(dimethylamino)pyrrolidin-1-yl]-2-methyl-5-nitrobiphenyl-3-carbonitrile (I-268) (1.40 g, 3.83 mmol), followed by stirring at room temperature for 1 hour. The insoluble matter was removed by filtration under suction, then the filtrate was diluted with ethyl acetate, washed with aqueous saturated sodium carbonate solution and saturated brine in that order, and dried over anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure, followed by drying with a vacuum pump to obtain the entitled compound (1.25 g, 97%) as a dark brown solid.

後処理

  1. customThe insoluble matter was removed by filtration under suction
  2. additionthe filtrate was diluted with ethyl acetate
  3. washwashed with aqueous saturated sodium carbonate solution and saturated brine in that order
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent was evaporated away under reduced pressure
  6. customby drying with a vacuum pump

出典と根拠

ORDレコード
ord-1a0f2bcf5dc94f82a80cbefce8556a45
出典データセット
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07737166B2

反応ノート

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