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1-Hydroxybenzotriazole → HCID 44545151, 화합물

HRID 2093393
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HRID 2093393 반응식
[O:1]1[CH2:6][CH2:5][N:4]([C:7]2[N:15]=[C:14]([C:16]3[CH:17]=[N:18][C:19]([NH2:22])=[N:20][CH:21]=3)[N:13]=[C:12]3[C:8]=2[N:9]=[CH:10][N:11]3[CH2:23][CH:24]2[CH2:29][CH2:28][NH:27][CH2:26][CH2:25]2)[CH2:3][CH2:2]1.C1C=CC2N([OH:39])N=NC=2C=1.C(N([CH:46]([CH3:48])C)CC)(C)C.Cl.CN(C)CCCN=C=NCC>CN(C=O)C.C(O)(=O)C>[NH2:22][C:19]1[N:20]=[CH:21][C:16]([C:14]2[N:13]=[C:12]3[C:8]([N:9]=[CH:10][N:11]3[CH2:23][CH:24]3[CH2:25][CH2:26][N:27]([C:46](=[O:39])[CH3:48])[CH2:28][CH2:29]3)=[C:7]([N:4]3[CH2:5][CH2:6][O:1][CH2:2][CH2:3]3)[N:15]=2)=[CH:17][N:18]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 58015216HCID 58015216, 화합물

생성물 1

HCID 44545151HCID 44545151, 화합물

시약·촉매·용매 2

HCID 176
Acetic Acid
용매
HCID 6228Dimethylformamide용매

실험 절차

5-(6-Morpholino-9-(piperidin-4-ylmethyl)-9H-purin-2-yl)pyrimidin-2-amine (75 mg) was reacted with excess acetic acid, 2 eq HOBT, 5 eq diisopropylethylamine and 2 eq N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride in 1 mL of DMF. Upon completion, the reaction was extracted with ethyl acetate and a saturated sodium bicarbonate solution. The organic layer was concentrated and purified via reverse phase HPLC to give 18.9 mg 107 as a white solid. MS (Q1) 438.3 (M)+

후처리

  1. extractionUpon completion, the reaction was extracted with ethyl acetate
  2. concentrationThe organic layer was concentrated
  3. custompurified via reverse phase HPLC

출처 및 근거

ORD 기록
ord-d6a36f146bc34020b535ddaa5e847f37
출처 데이터셋
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08445487B2

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