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

HRID 36908
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반응식

HRID 36908 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ae3db4f78f6546469875db280c67c323
출처 데이터셋
uspto-grants-1995_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05418248

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