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Triethylamine → 2-(Diaminomethyleneamino)-4-[2-(furfurylthio)acetylaminomethylthiazol-4-yl]thiazole

HRID 1491864
ノート
印刷プレビュー

反応式

HRID 1491864 の反応式
Cl.Cl.[NH2:3][CH2:4][C:5]1[S:6][CH:7]=[C:8]([C:10]2[N:11]=[C:12]([N:15]=[C:16]([NH2:18])[NH2:17])[S:13][CH:14]=2)[N:9]=1.[CH2:19]([S:25][CH2:26][C:27](O)=[O:28])[C:20]1[O:24][CH:23]=[CH:22][CH:21]=1.Cl.CN(C)CCCN=C=NCC.C(N(CC)CC)C>CN(C)C=O>[NH2:17][C:16](=[N:15][C:12]1[S:13][CH:14]=[C:10]([C:8]2[N:9]=[C:5]([CH2:4][NH:3][C:27](=[O:28])[CH2:26][S:25][CH2:19][C:20]3[O:24][CH:23]=[CH:22][CH:21]=3)[S:6][CH:7]=2)[N:11]=1)[NH2:18]
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 8471TriethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 3021476(Furfurylthio)acetic acidHCID 189538344-(2-Aminomethylthiazol-4-yl)-2-(diaminomethyleneamino)thiazole dihydrochloride

生成物 1

HCID 189538562-(Diaminomethyleneamino)-4-[2-(furfurylthio)acetylaminomethylthiazol-4-yl]thiazole収率 11%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A suspension of 4-(2-aminomethylthiazol-4-yl)-2-(diaminomethyleneamino)thiazole dihydrochloride (1.6 g), (furfurylthio)acetic acid (0.98 g), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (1.2 g) and triethylamine (1.0 g) in N,N-dimethylformamide (20 ml) was stirred with cooling on an ice-water bath for 2.5 hours. The solvent was removed under the reduced pressure. The residue was washed with water and then chromatographed on a silica gel column eluting with a mixture of chloroform and methanol (10:1). The appropriate fractions was collected and the solvent was removed under the reduced pressure. The residue was suspended in water (20 ml) and the mixture was alkalized to pH 11 with a saturated aqueous potassium carbonate solution. The resulting precipitate was collected by filtration. Recrystallization from a mixture of methanol and water afforded 2-(diaminomethyleneamino)-4-[2-(furfurylthio)acetylaminomethylthiazol-4-yl]thiazole (0.22 g).

後処理

  1. temperaturewith cooling on an ice-water bath for 2.5 hours
  2. customThe solvent was removed under the reduced pressure
  3. washThe residue was washed with water
  4. customchromatographed on a silica gel column
  5. washeluting with a mixture of chloroform and methanol (10:1)
  6. customThe appropriate fractions was collected
  7. customthe solvent was removed under the reduced pressure
  8. filtrationThe resulting precipitate was collected by filtration
  9. customRecrystallization
  10. additionfrom a mixture of methanol and water

出典と根拠

ORDレコード
ord-c8316d1772ee4b1c8fb40a3a7bf27bec
出典データセット
uspto-grants-1994_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05371097

反応ノート

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