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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Acetic Acid → 1-{1-[8-(4,5-Dimethyl-4H-1,2,4-triazol-3-yl)-9-methyl-9H-purin-6-yl]piperidin-4-yl}-1,3-dihydro-2H-benzimidazol-2-one

HRID 528049
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인쇄 미리보기

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HRID 528049 반응식
[CH3:1][N:2]1[C:10]([C:11]([NH:13][NH2:14])=O)=[N:9][C:8]2[C:3]1=[N:4][CH:5]=[N:6][C:7]=2[N:15]1[CH2:20][CH2:19][CH:18]([N:21]2[C:25]3[CH:26]=[CH:27][CH:28]=[CH:29][C:24]=3[NH:23][C:22]2=[O:30])[CH2:17][CH2:16]1.C(O[CH2:40][CH3:41])(OCC)(OCC)C.[CH3:42][NH2:43].C(O)(=O)C>CO.C(O)=O.C(#N)C.O.O1CCOCC1>[CH3:42][N:43]1[C:40]([CH3:41])=[N:14][N:13]=[C:11]1[C:10]1[N:2]([CH3:1])[C:3]2[C:8]([N:9]=1)=[C:7]([N:15]1[CH2:20][CH2:19][CH:18]([N:21]3[C:25]4[CH:26]=[CH:27][CH:28]=[CH:29][C:24]=4[NH:23][C:22]3=[O:30])[CH2:17][CH2:16]1)[N:6]=[CH:5][N:4]=2
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참가 물질

9

반응물 4

HCID 176Acetic AcidHCID 6329MethylamineHCID 66221Triethyl orthoacetateHCID 66799788HCID 66799788, 화합물

생성물 1

HCID 668022991-{1-[8-(4,5-Dimethyl-4H-1,2,4-triazol-3-yl)-9-methyl-9H-purin-6-yl]piperidin-4-yl}-1,3-dihydro-2H-benzimidazol-2-one

시약·촉매·용매 4

HCID 284
Formic Acid
용매
HCID 887Methanol용매
HCID 312751,4-Dioxane용매
HCID 18373917Acetonitrile--water (1/1)용매

반응 조건

온도
130 °C

실험 절차

Into an Ace pressure tube were placed 9-methyl-6-(4-(2-oxo-2,3-dihydro-1H-benzo[d]imidazol-1-yl)piperidin-1-yl)-9H-purine-8-carbohydrazide (115 mg, 0.28 mmol, 1.0 equiv), triethyl orthoacetate (80 μL, 0.43 mmol, 1.5 equiv), methylamine (775 μL, 2M in THF, 1.55 mmol, 5.5 equiv), and acetic acid (0.5 mL), and dioxane (1.5 mL). The tube was sealed and heated at 130° C. for 12 hours. The tube was cooled to room temperature and diluted with methanol (1 mL). The title compound was isolated by preparative reverse-phase HPLC (acetonitrile/water with 1% formic acid, 25-45% gradient). Purified fractions were combined, frozen, and lyophilized to yield 28 mg material. 1H-NMR (400 MHz, DMSO-d6): δ 10.81 (s, 1H), 8.31 (s, 1H), 7.12 (m, 1H), 6.87 (m, 3H), 5.5 (br s, 2H), 4.52 (m, 1H), 3.98 (d, 3H), 3.82 (s, 3H), 2.40 (s, 3H), 2.32 (dd, 2H), 1.82 (d, 2H); MS (EI) for C22H24N10O, found 445.3 (MH+).

후처리

  1. customThe tube was sealed
  2. temperatureThe tube was cooled to room temperature

출처 및 근거

ORD 기록
ord-88b9de65ebc24d4abaf8ffcb20879cd7
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09346807B2

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