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HCID 178483079, 화합물 → HCID 68846891, 화합물

HRID 1984908
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HRID 1984908 반응식
C(OC(=O)[NH:10][CH2:11][C@H:12]1[CH2:17][CH2:16][C@@H:15]([NH:18][C:19]2[N:28]=[C:27]([N:29]([CH3:31])[CH3:30])[C:26]3[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=3)[N:20]=2)[CH2:14][CH2:13]1)C1C=CC=CC=1>CO.[Pd]>[NH2:10][CH2:11][CH:12]1[CH2:13][CH2:14][CH:15]([NH:18][C:19]2[N:28]=[C:27]([N:29]([CH3:31])[CH3:30])[C:26]3[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=3)[N:20]=2)[CH2:16][CH2:17]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 178483079HCID 178483079, 화합물

생성물 1

HCID 68846891HCID 68846891, 화합물수율 83%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

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온도
50 °C

실험 절차

To a solution of cis-[4-(4-dimethylamino-quinazolin-2-ylamino)-cyclohexylmethyl]-carbamic acid benzyl ester obtained in step B of example 24 (12.1 g, 27.9 mmol) in MeOH (120 mL) was added 10% Pd/C (1.21 g). The mixture was stirred at 50° C. under hydrogen atmosphere for 19 hr, filtered, concentrated, and purified by flash chromatography (NH-silica gel, 66% EtOAc in hexane to 15% MeOH in chloroform) to give N2-(4-aminomethyl-cyclohexyl)-N4,N4-dimethyl-quinazoline-2,4-diamine (6.9 g, 83%) as a yellow solid.

후처리

  1. filtrationfiltered
  2. concentrationconcentrated
  3. custompurified by flash chromatography (NH-silica gel, 66% EtOAc in hexane to 15% MeOH in chloroform)

출처 및 근거

ORD 기록
ord-b5bf2f57bbea4696ae2ee0eefeee1f75
출처 데이터셋
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07544690B2

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