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Dimethyl Sulfoxide → N'-hydroxy-4-{3-[4-(3-hydroxypropyl)-1-piperidinyl]propoxy}benzamidine

HRID 644127
ノート
印刷プレビュー

反応式

HRID 644127 の反応式
CS(C)=O.[OH:5][CH2:6][CH2:7][CH2:8][CH:9]1[CH2:14][CH2:13][N:12]([CH2:15][CH2:16][CH2:17][O:18][C:19]2[CH:26]=[CH:25][C:22]([C:23]#[N:24])=[CH:21][CH:20]=2)[CH2:11][CH2:10]1.[NH2:27][OH:28].CC(O)C>O>[OH:28][N:27]=[C:23]([NH2:24])[C:22]1[CH:21]=[CH:20][C:19]([O:18][CH2:17][CH2:16][CH2:15][N:12]2[CH2:11][CH2:10][CH:9]([CH2:8][CH2:7][CH2:6][OH:5])[CH2:14][CH2:13]2)=[CH:26][CH:25]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 679Dimethyl SulfoxideHCID 787Hydroxylamine2 回HCID 3776IsopropanolHCID 68434383HCID 68434383、化合物

生成物 1

HCID 72264642N'-hydroxy-4-{3-[4-(3-hydroxypropyl)-1-piperidinyl]propoxy}benzamidine

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a dimethylsulfoxide (200 mL) solution of 18.7 g of 4-{3-[4-(3-hydroxypropyl)-1-piperidinyl]propoxy}benzonitrile was added 8.92 mL of a 50% hydroxylamine aqueous solution at room temperature, which was then stirred at the same temperature for 5 hours and 30 minutes. Thereto was added 8.92 mL of a 50% hydroxylamine aqueous solution at room temperature, which was stirred at the same temperature for 15 hours and 50 minutes. To the reaction mixture were added 2-propanol and water, which was then stirred at room temperature for one hour. The precipitate was collected by filtration and washed with water to provide 17.5 g of N′-hydroxy-4-{3-[4-(3-hydroxypropyl)-1-piperidinyl]propoxy}benzamidine as white solid form.

後処理

  1. stirringwhich was stirred at the same temperature for 15 hours and 50 minutes
  2. stirringwas then stirred at room temperature for one hour
  3. filtrationThe precipitate was collected by filtration
  4. washwashed with water

出典と根拠

ORDレコード
ord-4d04898d2a244b0283c2ab491337fb77
出典データセット
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07700623B2

反応ノート

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