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1-Methylpiperazine → HCID 69430551, 화합물

HRID 1593430
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HRID 1593430 반응식
CS([C:5]1[N:10]=[CH:9][C:8]([C:11]2[O:15][C:14]([C:16]3[CH:21]=[CH:20][N:19]=[CH:18][CH:17]=3)=[C:13]([C:22]3[CH:23]=[C:24]4[C:28](=[CH:29][CH:30]=3)[C:27](=[O:31])[CH2:26][CH2:25]4)[CH:12]=2)=[CH:7][N:6]=1)(=O)=O.[CH3:32][N:33]1[CH2:38][CH2:37][NH:36][CH2:35][CH2:34]1>CN(C)C=O>[CH3:32][N:33]1[CH2:38][CH2:37][N:36]([C:5]2[N:10]=[CH:9][C:8]([C:11]3[O:15][C:14]([C:16]4[CH:21]=[CH:20][N:19]=[CH:18][CH:17]=4)=[C:13]([C:22]4[CH:23]=[C:24]5[C:28](=[CH:29][CH:30]=4)[C:27](=[O:31])[CH2:26][CH2:25]5)[CH:12]=3)=[CH:7][N:6]=2)[CH2:35][CH2:34]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 531671-MethylpiperazineHCID 69430943HCID 69430943, 화합물

생성물 1

HCID 69430551HCID 69430551, 화합물수율 57%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
90 °C

실험 절차

A solution of the product from Step 6 (0.15 g, 0.35 mmol) in dry dimethylformamide (2 ml) was treated with N-methylpiperazine (0.077 ml, 0.70 mmol) and heated at 90° C. for 2 hours. After cooling to room temperature the reaction mixture was applied to a SCX column and washed with methanol then a mixture of 0.880 ammonia/methanol (1:9). The basic fractions were combined and chromatographed on silica gel eluting with 0.880 ammonia/methanol/dichloromethane solution (0.5:4.5:95) to afford the title compound (0.09 g, 57%); MS(ES+) m/e 452 [M+H]+.

후처리

  1. temperatureAfter cooling to room temperature the reaction mixture
  2. washwashed with methanol
  3. additiona mixture of 0.880 ammonia/methanol (1:9)
  4. customchromatographed on silica gel eluting with 0.880 ammonia/methanol/dichloromethane solution (0.5:4.5:95)

출처 및 근거

ORD 기록
ord-71720ae5ea994d6c8443fd54217af460
출처 데이터셋
uspto-grants-2007_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07297694B2

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