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Water → HCID 68778456, 화합물

HRID 2263008
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HRID 2263008 반응식
Cl[C:2]1[S:6][N:5]=[C:4]([N:7]2[CH2:12][CH2:11][CH:10]([OH:13])[CH2:9][CH2:8]2)[N:3]=1.FC(F)(F)C(O)=O.[O:21]1[C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][C:24]=2[C:23]([NH:30][C:31]([N:33]2[CH2:38][CH2:37][NH:36][CH2:35][CH2:34]2)=[O:32])=[N:22]1.C(N(CC)CC)C.O>CN(C)C=O>[O:21]1[C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][C:24]=2[C:23]([NH:30][C:31]([N:33]2[CH2:38][CH2:37][N:36]([C:2]3[S:6][N:5]=[C:4]([N:7]4[CH2:12][CH2:11][CH:10]([OH:13])[CH2:9][CH2:8]4)[N:3]=3)[CH2:35][CH2:34]2)=[O:32])=[N:22]1
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참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 68778018N-1,2-Benzisoxazol-3-ylpiperazine-1-carboxamide trifluoroacetateHCID 68778582HCID 68778582, 화합물

생성물 1

HCID 68778456HCID 68778456, 화합물수율 33.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide
용매

실험 절차

To a solution of 1-(5-chloro-1,2,4-thiadiazol-3-yl)piperidin-4-ol (153 mg, 0.555 mmol) and N-1,2-benzisoxazol-3-ylpiperazine-1-carboxamide trifluoroacetate (200 mg, 0.555 mmol) in N,N-dimethylformamide (2 ml) was added triethylamine (0.387 ml, 2.78 mmol) at room temperature, and the mixture was stirred at room temperature for 1 hour. The reaction mixture was poured to water, and a solid was separated by filtration and washed with water, which was recrystallized from a mixed solvent of tetrahydrofuran and ethyl acetate to give 79.0 mg (33.2%) of the desired product as a solid.

후처리

  1. customa solid was separated by filtration
  2. washwashed with water, which
  3. customwas recrystallized from a mixed solvent of tetrahydrofuran and ethyl acetate

출처 및 근거

ORD 기록
ord-0ca600ffad884f3186ba9388098cf18d
출처 데이터셋
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07851473B2

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