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Ammonia → 2-(5-Methylthien-2-yl)imidazo[2,1-b]benzothiazole-3-acetamide

HRID 36908
ノート
印刷プレビュー

反応式

HRID 36908 の反応式
[CH3:1][C:2]1[S:6][C:5]([C:7]2[N:8]=[C:9]3[N:13]([C:14]=2[CH2:15][C:16](O)=[O:17])[C:12]2[CH:19]=[CH:20][CH:21]=[CH:22][C:11]=2[S:10]3)=[CH:4][CH:3]=1.[NH3:23]>O1CCCC1>[CH3:1][C:2]1[S:6][C:5]([C:7]2[N:8]=[C:9]3[N:13]([C:14]=2[CH2:15][C:16]([NH2:23])=[O:17])[C:12]2[CH:19]=[CH:20][CH:21]=[CH:22][C:11]=2[S:10]3)=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 222AmmoniaHCID 152338102-(5-Methylthien-2-yl)imidazo[2,1-b]benzothiazole-3-acetic acid

生成物 1

HCID 199367262-(5-Methylthien-2-yl)imidazo[2,1-b]benzothiazole-3-acetamide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

1.6 g (0.005 mole) of 2-(5-methylthien-2-yl)imidazo[2,1-b]-benzothiazole-3-acetic acid are treated, at room temperature, with 0.85 g (0.005 mole) of N,N'-carbonyldiimidazole in 30 ml of anhydrous tetrahydrofuran for 3 h 30 min. The mixture is cooled using an ice bath, an excess of ammonia in 10 ml of anhydrous tetrahydrofuran cooled to -10° C. is added, and the mixture is stirred for 4 h at room temperature. The solvent is evaporated under reduced pressure, the solid is collected by filtration, it is washed with water up to neutral pH, then with ethanol, and finally with ethyl ether. After recrystallization from methanol, 1 g of a beige compound is obtained. Melting point: 243°-245° C.

後処理

  1. temperatureThe mixture is cooled
  2. additionis added
  3. customThe solvent is evaporated under reduced pressure
  4. filtrationthe solid is collected by filtration, it
  5. washis washed with water up to neutral pH
  6. customAfter recrystallization from methanol

出典と根拠

ORDレコード
ord-ae3db4f78f6546469875db280c67c323
出典データセット
uspto-grants-1995_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05418248

反応ノート

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