Cyanuric chloride → HCID 58101013, 화합물

HRID 222624노트

반응식

HRID 222624 반응식
ClC1N=C(Cl)N=C(Cl)N=1.[CH2:10]([O:17][C:18]1[C:23](=[O:24])[N:22]2[CH:25]=[C:26]([CH3:29])[CH:27]=[CH:28][C:21]2=[N:20][C:19]=1[CH:30]=[N:31]O)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.C(OCC)(=O)C>CN(C)C=O>[CH2:10]([O:17][C:18]1[C:23](=[O:24])[N:22]2[CH:25]=[C:26]([CH3:29])[CH:27]=[CH:28][C:21]2=[N:20][C:19]=1[C:30]#[N:31])[C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1

참가 물질

5

반응물 3

HCID 7954Cyanuric chlorideHCID 8857Ethyl AcetateHCID 76655923HCID 76655923, 화합물

생성물 1

HCID 58101013HCID 58101013, 화합물수율 60.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

Trichloro-1,3,5-triazine (576 mg, 3.15 mmol) was dissolved in anhydrous N,N-dimethylformamide (DMF) (1 mL) and stirred at room temperature for 30 min. To this solution was added dropwise a solution of the product from Example 11.1 (927 mg, 3 mmol) in DMF (5 mL). The mixture was kept at room temperature for 2 h, then ethyl acetate (50 mL) was added and the organic phase separated and washed with brine, dried (Na2SO4) and concentrated in vacuo. Purification by short flash chromatography afforded the desired compound (530 mg, 60.7%).

후처리

  1. waitThe mixture was kept at room temperature for 2 h
  2. customthe organic phase separated
  3. washwashed with brine
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated in vacuo
  6. customPurification by short flash chromatography

출처 및 근거

ORD 기록
ord-58980e01b5e744c0976b07bbe61300e0
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08207334B2

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