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Water → 6-[(4-Chlorophenyl)-(1,2,4-triazol-1-yl)methyl]-1-methylbenzotriazole

HRID 1376825
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HRID 1376825 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:13]2[CH:14]=[CH:15][C:16]3[N:20]=[N:19][N:18]([CH3:21])[C:17]=3[CH:22]=2)[NH:9][NH:10][CH:11]=O)=[CH:4][CH:3]=1.C(O)(=O)C.[CH:27](=N)[NH2:28].O>CO>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([N:9]2[CH:27]=[N:28][CH:11]=[N:10]2)[C:13]2[CH:14]=[CH:15][C:16]3[N:20]=[N:19][N:18]([CH3:21])[C:17]=3[CH:22]=2)=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 160693Formamidine acetateHCID 229185642-[(4-chlorophenyl)(1-methyl-1H-benzotriazol-6-yl)methyl]hydrazinecarboxaldehyde

생성물 1

HCID 607966-[(4-Chlorophenyl)-(1,2,4-triazol-1-yl)methyl]-1-methylbenzotriazole수율 67.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 5 g of intermediate 7-a, 8.2 g of methanimidamide monoacetate in 32 ml of methanol was refluxed for 3 days. To the warm reaction mixture there were added 32 ml of water and the resulting mixture was stirred for two hours. The precipitate was filtered off and washed with 2-propanol. The precipitate was dried in vacuo, yielding 3.45 g (67%) of (+)-6-[(4-chlorophenyl)-(1H-1,2,4-triazol-1-yl)methyl]-1-methyl-1H-benzotriazole (comp. 1-e); enantiomeric excess: 97.4%.

후처리

  1. temperaturewas refluxed for 3 days
  2. customTo the warm reaction mixture there
  3. filtrationThe precipitate was filtered off
  4. washwashed with 2-propanol
  5. customThe precipitate was dried in vacuo

출처 및 근거

ORD 기록
ord-5bbe0d60a6b34695a6b8ac3af26246dc
출처 데이터셋
uspto-grants-1997_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05663354

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