Trityl chloride → Dimethyl 1-trityl-3,5-pyrazoledicarboxylate

HRID 66237

반응식

HRID 66237 반응식
[CH3:1][O:2][C:3]([C:5]1[CH:9]=[C:8]([C:10]([O:12][CH3:13])=[O:11])[NH:7][N:6]=1)=[O:4].[H-].[Na+].[H][H].[C:18]1([C:24](Cl)([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1>O.CN(C=O)C>[C:18]1([C:24]([C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=2)([C:31]2[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=2)[N:7]2[C:8]([C:10]([O:12][CH3:13])=[O:11])=[CH:9][C:5]([C:3]([O:2][CH3:1])=[O:4])=[N:6]2)[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1

참가 물질

7

반응물 4

HCID 6456Trityl chlorideHCID 24758Sodium hydrideHCID 14844913,5-dimethyl 1H-pyrazole-3,5-dicarboxylateHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 12377531Dimethyl 1-trityl-3,5-pyrazoledicarboxylate

시약·촉매·용매 2

HCID 962Water용매2회HCID 6228Dimethylformamide용매3회

실험 절차

To a solution of 1.84 g. (10 mmol) of 3,5-pyrazoledicarboxylic acid dimethyl ester* in 15 ml. of DMF, stirred at 0° under argon, was added 480 mg. (10 mmol) of 50% NaH (suspension in mineral oil). After the evolution of hydrogen had ceased, 2.7 g. (10 mmol) of triphenylmethyl chloride in 20 ml. of DMF was added dropwise. The mixture was allowed to warm to room temperature, stirred 1.5 hours, poured into H2O, and the resulting precipitate filtered. After recrystallization from 2-ethoxyethanol-H2O, there was obtained the end product. The analytical sample was obtained as colorless needles by recrystallization from DMF--H2O; mp 212°-213.5°.

후처리

  1. additionwas added 480 mg
  2. filtrationthe resulting precipitate filtered
  3. customAfter recrystallization from 2-ethoxyethanol-H2O
  4. customthere was obtained the end product

출처 및 근거

ORD 기록
ord-4cb4b126c5764aeda3984b513850da27
출처 데이터셋
uspto-grants-1978_12
특허 번호
US04130716

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