Water → HCID 178488013, 화합물

HRID 1007308노트

반응식

HRID 1007308 반응식
C(N(CC)C(C)C)(C)C.[Cl:10][C:11]1[CH:19]=[CH:18][C:14]([C:15](Cl)=[O:16])=[CH:13][CH:12]=1.[C:20]([O:24][C:25]([NH:27][C:28]([NH:37][C@@H:38]1[CH2:43][CH2:42][CH2:41][CH2:40][C@@H:39]1[NH:44][C:45]1[C:54]2[C:49](=[CH:50][CH:51]=[C:52]([O:55][CH3:56])[CH:53]=2)[N:48]=[C:47]([NH2:57])[N:46]=1)=[N:29][C:30]([O:32][C:33]([CH3:36])([CH3:35])[CH3:34])=[O:31])=[O:26])([CH3:23])([CH3:22])[CH3:21].O>C(Cl)Cl.CN(C)C1C=CN=CC=1>[C:33]([O:32][C:30]([NH:29][C:28]([NH:37][C@@H:38]1[CH2:43][CH2:42][CH2:41][CH2:40][C@@H:39]1[NH:44][C:45]1[C:54]2[C:49](=[CH:50][CH:51]=[C:52]([O:55][CH3:56])[CH:53]=2)[N:48]=[C:47]([NH:57][C:15](=[O:16])[C:14]2[CH:18]=[CH:19][C:11]([Cl:10])=[CH:12][CH:13]=2)[N:46]=1)=[N:27][C:25]([O:24][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:26])=[O:31])([CH3:34])([CH3:35])[CH3:36]

참가 물질

7

반응물 4

HCID 962WaterHCID 85014-Chlorobenzoyl chlorideHCID 81531DiisopropylethylamineHCID 178488017HCID 178488017, 화합물

생성물 1

HCID 178488013HCID 178488013, 화합물

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매2회

실험 절차

A solution of 366 mg of N,N-diisopropylethylamine in 10 mL of methylene chloride was combined with 60 mg of 4-dimethylaminopyridine and 0.156 mL of 4-chlorobenzoyl chloride. This was treated dropwise with a solution of 500 mg of (1R,2S)-N-[N,N′-bis(tert-butoxycarbonyl)]amidino-2-(2-amino-6-methoxyquinazolin-4-yl)aminocyclohexylamine in 10 mL of methylene chloride, and stirred at room temperature for 3 hours. The reaction solution was combined with water, extracted with methylene chloride, and dried. After the solvent was distilled off, the residue was purified by column chromatography on silica gel (chloroform:methanol=30:1) to obtain 560 mg of the desirable compound.

후처리

  1. extractionextracted with methylene chloride
  2. customdried
  3. distillationAfter the solvent was distilled off
  4. customthe residue was purified by column chromatography on silica gel (chloroform:methanol=30:1)

출처 및 근거

ORD 기록
ord-73f05044f3e34625bf0c8c86d4582965
출처 데이터셋
uspto-grants-2004_09
특허 번호
US06794389B2

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