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Benzyl Alcohol → HCID 178508946, 화합물

HRID 2081799
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HRID 2081799 반응식
[Na].[CH2:2]([OH:9])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.Cl[C:11]1[C:12]2[NH:20][N:19]=[N:18][C:13]=2[N:14]=[C:15]([NH2:17])[N:16]=1>O>[C:3]1([CH2:2][O:9][C:11]2[C:12]3[NH:20][N:19]=[N:18][C:13]=3[N:14]=[C:15]([NH2:17])[N:16]=2)[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 244Benzyl AlcoholHCID 5360545Sodium2회HCID 178508438HCID 178508438, 화합물

생성물 1

HCID 178508946HCID 178508946, 화합물수율 61.4%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Sodium metal (3.7 g, 0.162 mol) was added in pieces to benzyl alcohol (117 ml, 1.13 mol) under nitrogen over 20 minutes. The reaction was then heated to 80° for 90 minutes. All of the sodium metal dissolved, and the reaction was left at room temperature for 16 hours. 7-Chloro-1H-1,2,3triazolo[4,5-d]pyrimidin-5-amine (9.23 g. 0.0541 mol) was then added, and the reaction was heated to 60° for 5 hours. The reaction was cooled and left at 5° for 16 hours. Water (500 ml) was added to dissolve the precipitate and then the mixture was extracted with ether (3×200 ml). The pH of the water layer was lowered to 7.0 with concentrated HCl and then to 5.5 with 1N HCl. The precipitate was filtered and dried at room temperature over P2O5 in vacuo to give 8.05 g of desired product.

후처리

  1. temperatureThe reaction was then heated to 80° for 90 minutes
  2. temperaturethe reaction was heated to 60° for 5 hours
  3. temperatureThe reaction was cooled
  4. waitleft at 5° for 16 hours
  5. dissolutionto dissolve the precipitate
  6. extractionthe mixture was extracted with ether (3×200 ml)
  7. filtrationThe precipitate was filtered
  8. dry with materialdried at room temperature over P2O5 in vacuo

출처 및 근거

ORD 기록
ord-835c9b615e6249538ba00176c0114b24
출처 데이터셋
uspto-grants-1993_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05185459

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