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Water → HCID 58098670, 화합물

HRID 384249
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HRID 384249 반응식
N1(O[C:11]2[N:16]=[C:15]([NH:17][CH2:18][CH:19]3[CH2:24][CH2:23][CH2:22][N:21]([C:25]([O:27][CH2:28][C:29]4[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=4)=[O:26])[CH2:20]3)[C:14]([C:35](=[O:37])[NH2:36])=[CH:13][N:12]=2)C2C=CC=CC=2N=N1.[NH2:38][C:39]1[CH:40]=[C:41]([CH:46]=[CH:47][CH:48]=1)[NH:42][C:43](=[O:45])[CH3:44].CC1C=CC(S(O)(=O)=O)=CC=1.O>O1CCOCC1.CCOC(C)=O>[C:43]([NH:42][C:41]1[CH:40]=[C:39]([NH:38][C:11]2[N:16]=[C:15]([NH:17][CH2:18][CH:19]3[CH2:24][CH2:23][CH2:22][N:21]([C:25]([O:27][CH2:28][C:29]4[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=4)=[O:26])[CH2:20]3)[C:14]([C:35](=[O:37])[NH2:36])=[CH:13][N:12]=2)[CH:48]=[CH:47][CH:46]=1)(=[O:45])[CH3:44]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 6101p-Toluenesulfonic acidHCID 7604m-AminoacetanilideHCID 58014797HCID 58014797, 화합물

생성물 1

HCID 58098670HCID 58098670, 화합물수율 68.6%

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매
HCID 31275
1,4-Dioxane
용매

실험 절차

A mixture of benzyl 3-((2-(1H-benzo[d][1,2,3]triazol-1-yloxy)-5-carbamoylpyrimidin-4-ylamino)methyl)piperidine-1-carboxylate (582 mg, 1.16 mmol), 3′-amino-acetanilide (210 mg, 1.40 mmol) and pTsOH (220 mg, 1.16 mmol) in dioxane (10 mL) was stirred at 100 C for 4 h. Water and EtOAc were added. The organic phase was separated, washed with 1N HCl. During the washing white solids precipitated out, which were collected to give the titled compound (412 mg). MS 518.5 (M+H); UV 201.6, 249.8 nm.

후처리

  1. customThe organic phase was separated
  2. washwashed with 1N HCl
  3. customDuring the washing white solids precipitated out
  4. customwhich were collected

출처 및 근거

ORD 기록
ord-800bb623d00449e38a08f307663d78c1
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08367689B2

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