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Dimethylamine → HCID 18768058, 화합물

HRID 480011
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HRID 480011 반응식
[CH3:1][NH:2][CH3:3].[NH:4]([C:11]1[C:16]([Br:17])=[CH:15][N:14]=[C:13]([NH:18][C:19]2[CH:24]=[CH:23][C:22]([NH:25][C:26](=[O:30])[CH2:27][CH2:28]Cl)=[CH:21][CH:20]=2)[N:12]=1)[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1>O1CCCC1.CN(C=O)C.C(Cl)Cl>[NH:4]([C:11]1[C:16]([Br:17])=[CH:15][N:14]=[C:13]([NH:18][C:19]2[CH:24]=[CH:23][C:22]([NH:25][C:26](=[O:30])[CH2:27][CH2:28][N:2]([CH3:3])[CH3:1])=[CH:21][CH:20]=2)[N:12]=1)[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 674DimethylamineHCID 18768057HCID 18768057, 화합물

생성물 1

HCID 18768058HCID 18768058, 화합물수율 9%

시약·촉매·용매 3

HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매HCID 8028Tetrahydrofuran용매

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온도
80 °C

실험 절차

A solution of dimethylamine in tetrahydrofuran (2.0M; 4 ml) was added to a solution of 4-anilino-5-bromo-2-[4-(3-chloropropionamido)anilino]pyrimidine (Method 37; 60 mg, 0.135 mmol) in DMF (0.2 ml). The solution was heated at 80° C. for 1 hour, diluted with DCM (4 ml) and loaded onto a Varian Mega Bond Elut column. Elution with 0-10% 2.0M methanolic ammonia solution in DCM gave the product (5.4 mg, 9%). MS (MH+): 455, 457; HPLC (RT): 2.70.

후처리

  1. washElution with 0-10% 2.0M methanolic ammonia solution in DCM

출처 및 근거

ORD 기록
ord-364e4acbe6af462a8d5c3c77159df2be
출처 데이터셋
uspto-grants-2003_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06649608B2

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