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Triethylamine → 4-(benzyloxy)-2-(1H-pyrazol-1-yl)pyrimidine-5-carboxylic acid

HRID 1470311
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HRID 1470311 반응식
NC1C(O)=NC(N2C=CC=N2)=NC=1.[CH2:14]([O:21][C:22]1[C:27]([C:28]([OH:30])=[O:29])=[CH:26][N:25]=[C:24]([N:31]2[CH:35]=[CH:34][CH:33]=[N:32]2)[N:23]=1)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.C(Cl)(=O)C(Cl)=O.CCN(CC)CC.[N-:49]=[N+:50]=[N-:51].[Na+]>ClCCl.CN(C=O)C.O>[CH2:14]([O:21][C:22]1[C:27]([C:28]([OH:30])=[O:29])=[CH:26][N:25]=[C:24]([N:31]2[CH:35]=[CH:34][CH:33]=[N:32]2)[N:23]=1)[C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1.[N:49]([C:28]([C:27]1[C:22]([O:21][CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[N:23][C:24]([N:31]2[CH:35]=[CH:34][CH:33]=[N:32]2)=[N:25][CH:26]=1)=[O:29])=[N+:50]=[N-:51]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 5

HCID 8471TriethylamineHCID 33557Sodium AzideHCID 65578Oxalyl chlorideHCID 674594834-(benzyloxy)-2-(1H-pyrazol-1-yl)pyrimidine-5-carboxylic acid2회HCID 178508031HCID 178508031, 화합물

생성물 2

HCID 674594834-(benzyloxy)-2-(1H-pyrazol-1-yl)pyrimidine-5-carboxylic acid
HCID 89372972
Azido(4-(benzyloxy)-2-(1H-pyrazol-1-yl)pyrimidin-5-yl)methanone

시약·촉매·용매 3

HCID 6228Dimethylformamide촉매HCID 962Water용매2회HCID 6344Dichloromethane용매

실험 절차

4-(benzyloxy)-2-(1H-pyrazol-1-yl)pyrimidine-5-carboxylic acid (3-c) was synthesized in a manner outlined in Steps A through Step C of the synthesis of Intermediate 3-e. To a solution of 4-(benzyloxy)-2-(1H-pyrazol-1-yl)pyrimidine-5-carboxylic acid, 3-c, (500 mg, 1.69 mmol) in dry dichloromethane (10 ml) was added dropwise oxalyl chloride (0.29 ml, 3.38 mmol) at 0° C. and a catalytic amount of DMF (3-5 drops). The mixture was stirred at room temperature for 3 hours. Then the mixture was concentrated under vacuum and the residue was dissolved in acetone (10 ml). Et3N (205 mg, 2.03 mmol) was added at 0° C. and the mixture was stirred for 5 mins before sodium azide (988 mg, 15.2 mmol) in water (1 ml) was added. The resulting mixture was stirred at room temperature for 1 h. Subsequently, the mixture was diluted with water and filtered. The solid was washed with water (5-10 ml) and then taken into approximately 20-30 mL of dichloromethane. The organic layer was dried over sodium sulfate and concentrated under vacuum to provide compound 5-a as a solid (130 mg) which was used in Step B without any further purification. (M+H)+=322.

후처리

  1. concentrationThen the mixture was concentrated under vacuum
  2. dissolutionthe residue was dissolved in acetone (10 ml)
  3. additionwas added
  4. stirringThe resulting mixture was stirred at room temperature for 1 h
  5. filtrationfiltered
  6. washThe solid was washed with water (5-10 ml)
  7. dry with materialThe organic layer was dried over sodium sulfate
  8. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-84d984c822014756886b7e8c5f7aca90
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09006433B2

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