Acetic Anhydride → HCID 75238442, 화합물

HRID 1474477노트

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HRID 1474477 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 75238442HCID 75238442, 화합물수율 32.3%

시약·촉매·용매 1

HCID 962Water용매

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온도
90 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e27933fe8c66459e99a87bde895885b5
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09018238B2

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