Isobutyramide → HCID 57657265、化合物

HRID 244814

反応式

HRID 244814 の反応式
Br[C:2]1[CH:3]=[CH:4][C:5]2[C:6]3[N:15]([CH2:16][C:17]([OH:20])([CH3:19])[CH3:18])[C:14]([CH2:21][O:22][CH2:23][CH3:24])=[N:13][C:7]=3[C:8]([NH2:12])=[N:9][C:10]=2[CH:11]=1.BrC1C=CC2C3N(CCCOC(C)C)C(COCC)=NC=3C=NC=2C=1.[CH2:50]([S:52]([NH2:55])(=[O:54])=[O:53])[CH3:51].C(N)(=O)C(C)C>>[NH2:12][C:8]1[C:7]2[N:13]=[C:14]([CH2:21][O:22][CH2:23][CH3:24])[N:15]([CH2:16][C:17]([OH:20])([CH3:19])[CH3:18])[C:6]=2[C:5]2[CH:4]=[CH:3][C:2]([NH:55][S:52]([CH2:50][CH3:51])(=[O:54])=[O:53])=[CH:11][C:10]=2[N:9]=1

参加物

5

反応物 4

HCID 68424IsobutyramideHCID 73702EthanesulfonamideHCID 219842117-bromo-2-ethoxymethyl-1-(2-hydroxy-2-methylpropyl)-1H-imidazo[4,5-c]quinolin-4-amineHCID 673819647-Bromo-2-ethoxymethyl-1-(isopropoxypropyl)-1H-imidazo[4,5-c]quinoline

生成物 1

HCID 57657265HCID 57657265、化合物

実験手順

The general method described in Part A of Example 3 was followed using 7-bromo-2-ethoxymethyl-1-(2-hydroxy-2-methylpropyl)-1H-imidazo[4,5-c]quinolin-4-amine (U.S. Patent Application Publication No. US 2004/0147543, Examples 125-135) in lieu of 7-bromo-2-ethoxymethyl-1-(3-isopropoxypropyl)-1H-imidazo[4,5-c]quinoline and ethanesulfonamide in lieu of isobutyramide. Purification using a HORIZON HPFC system (silica cartridge, eluting with a linear gradient of 2-25% CMA in chloroform), followed by recrystallization from acetonitrile afforded 0.108 g of N-[4-amino-2-ethoxymethyl-1-(2-hydroxy-2-methylpropyl)-1H-imidazo[4,5-c]quinolin-7-yl]ethanesulfonamide as white crystals, mp 124.0-127.0° C.

後処理

  1. customPurification
  2. washeluting with a linear gradient of 2-25% CMA in chloroform),
  3. customfollowed by recrystallization from acetonitrile

出典と根拠

ORDレコード
ord-f7395c6d0b464896a2eb1c53acdd9e27
出典データセット
uspto-grants-2014_02
特許番号
US08658666B2

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