Acetic Anhydride → HCID 75238442、化合物

HRID 1474477ノート

反応式

HRID 1474477 の反応式
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]([NH:8][CH2:9][C:10]([OH:12])=[O:11])=O.[CH3:13][N:14]([CH3:23])[C:15]1[C:20]([CH:21]=O)=[CH:19][CH:18]=[CH:17][N:16]=1.C([O-])(=O)C.[Na+].C(OC(=O)C)(=O)C>O>[CH3:13][N:14]([CH3:23])[C:15]1[C:20]([CH:21]=[C:9]2[C:10](=[O:11])[O:12][C:6]([C:2]3[S:1][CH:5]=[CH:4][CH:3]=3)=[N:8]2)=[CH:19][CH:18]=[CH:17][N:16]=1

参加物

6

反応物 4

HCID 7918Acetic AnhydrideHCID 517045Sodium AcetateHCID 679227((2-Thienylcarbonyl)amino)acetic acidHCID 64866102-(Dimethylamino)pyridine-3-carbaldehyde

生成物 1

HCID 75238442HCID 75238442、化合物収率 32.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
90 °C

実験手順

To a screw-capped test tube, N-(2-thienylcarbonyl)glycine (56 mg, 0.3 mmol), 2-(dimethylamino)-3-pyridinecarboxaldehyde (50 mg, 0.3 mmol), sodium acetate (25 mg, 0.3 mmol) and acetic anhydride (0.3 mL) were added. The test tube was sealed, and it was then stirred at an external temperature of 90° C. Three hours later, the temperature of the reaction solution was returned to room temperature, and water (1.5 mL) was then added thereto. The obtained mixture was stirred at the same temperature as described above for 1.5 hours. Thereafter, the precipitated crystal was collected by filtration, and it was washed with water (5 mL) and was then dried under reduced pressure, so as to obtain 29 mg of the above-captioned compound.

後処理

  1. customThe test tube was sealed
  2. customThree hours
  3. customwas returned to room temperature
  4. stirringThe obtained mixture was stirred at the same temperature
  5. customas described above for 1.5 hours
  6. filtrationThereafter, the precipitated crystal was collected by filtration, and it
  7. washwas washed with water (5 mL)
  8. customwas then dried under reduced pressure

出典と根拠

ORDレコード
ord-e27933fe8c66459e99a87bde895885b5
出典データセット
uspto-grants-2015_04
特許番号
US09018238B2

反応ノート

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