Water → HCID 178488013、化合物

HRID 1007308ノート

反応式

HRID 1007308 の反応式
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]

参加物

7

反応物 4

HCID 962WaterHCID 85014-Chlorobenzoyl chlorideHCID 81531DiisopropylethylamineHCID 178488017HCID 178488017、化合物

生成物 1

HCID 178488013HCID 178488013、化合物

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒2 回

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-73f05044f3e34625bf0c8c86d4582965
出典データセット
uspto-grants-2004_09
特許番号
US06794389B2

反応ノート

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