Toluene → N-(5-ethyl-1,3,4-thiadiazol-2-yl)butanamide

HRID 2256201ノート

反応式

HRID 2256201 の反応式
[NH2:1][C:2]1[S:3][C:4]([CH2:7][CH3:8])=[N:5][N:6]=1.C1(C)C=CC=CC=1.[C:16](Cl)(=[O:20])[CH2:17][CH2:18][CH3:19].C(=O)(O)[O-].[Na+]>C(OCC)(=O)C.C(N(CC)CC)C>[C:16]([NH:1][C:2]1[S:3][C:4]([CH2:7][CH3:8])=[N:5][N:6]=1)(=[O:20])[CH2:17][CH2:18][CH3:19]

参加物

7

反応物 4

HCID 1140TolueneHCID 8855Butyryl chlorideHCID 264442-Amino-5-ethyl-1,3,4-thiadiazoleHCID 516892Sodium Bicarbonate

生成物 1

HCID 693955N-(5-ethyl-1,3,4-thiadiazol-2-yl)butanamide収率 80.4%

試薬・触媒・溶媒 2

HCID 8471Triethylamine溶媒HCID 8857Ethyl Acetate溶媒

実験手順

2-Amino-5-ethyl-1,3,4-thiadiazole (0.5 g) was added to a mixture of toluene (5 ml) and triethylamine (0.4 g). With stirring, butyryl chloride (0.5 g) was added to the suspension at room temperature. After stirring for 2 hours, aqueous sodium bicarbonate solution and ethyl acetate were added to the reaction mixture. The organic layer was separated and washed with water several times. The precipitated crystals and the organic layer were combined and the solvent was concentrated to 5 ml. The precipitated crystals were filtrated and dried. The title compound (0.62 g) was obtained.

後処理

  1. stirringAfter stirring for 2 hours
  2. customThe organic layer was separated
  3. washwashed with water several times
  4. concentrationthe solvent was concentrated to 5 ml
  5. filtrationThe precipitated crystals were filtrated
  6. customdried

出典と根拠

ORDレコード
ord-3677fff9712043b1a5b3ea709ac8e1e9
出典データセット
uspto-grants-1997_08
特許番号
US05654322

反応ノート

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