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Lithium Hydroxide → 6-(6-(3-Ethylureido)-4-(4-(trifluoromethyl)thiazol-2-yl)pyridin-3-yl)-1-(1-(2-morpholinoethyl)piperidin-3-yl)-4-oxo-1,4-dihydro-1,8-naphthyridine-3-carboxylic acid

HRID 1047129
ノート
印刷プレビュー

反応式

HRID 1047129 の反応式
[CH2:1]([NH:3][C:4](=[O:24])[NH:5][C:6]1[N:11]=[CH:10][C:9](B(O)O)=[C:8]([C:15]2[S:16][CH:17]=[C:18]([C:20]([F:23])([F:22])[F:21])[N:19]=2)[CH:7]=1)[CH3:2].Br[C:26]1[CH:27]=[C:28]2[C:33](=[N:34][CH:35]=1)[N:32]([C@H:36]1[CH2:41][CH2:40][CH2:39][N:38]([CH2:42][CH2:43][N:44]3[CH2:49][CH2:48][O:47][CH2:46][CH2:45]3)[CH2:37]1)[CH:31]=[C:30]([C:50]([O:52]CC)=[O:51])[C:29]2=[O:55].C([O-])([O-])=O.[Cs+].[Cs+].[Li+].[OH-]>O1CCOCC1.O.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH2:1]([NH:3][C:4](=[O:24])[NH:5][C:6]1[N:11]=[CH:10][C:9]([C:26]2[CH:27]=[C:28]3[C:33](=[N:34][CH:35]=2)[N:32]([CH:36]2[CH2:41][CH2:40][CH2:39][N:38]([CH2:42][CH2:43][N:44]4[CH2:45][CH2:46][O:47][CH2:48][CH2:49]4)[CH2:37]2)[CH:31]=[C:30]([C:50]([OH:52])=[O:51])[C:29]3=[O:55])=[C:8]([C:15]2[S:16][CH:17]=[C:18]([C:20]([F:23])([F:22])[F:21])[N:19]=2)[CH:7]=1)[CH3:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 3939Lithium HydroxideHCID 10796Cesium carbonateHCID 594161896-(3-Ethylureido)-4-(4-(trifluoromethyl)thiazol-2-yl)pyridin-3-ylboronic acid2 回HCID 69621275(S)-ethyl 6-bromo-1-(1-(2-morpholinoethyl)piperidin-3-yl)-4-oxo-1,4-dihydro-1,8-naphthyridine-3-carboxylate2 回

生成物 1

HCID 68747251
6-(6-(3-Ethylureido)-4-(4-(trifluoromethyl)thiazol-2-yl)pyridin-3-yl)-1-(1-(2-morpholinoethyl)piperidin-3-yl)-4-oxo-1,4-dihydro-1,8-naphthyridine-3-carboxylic acid

試薬・触媒・溶媒 3

HCID 178418397HCID 178418397、化合物触媒HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

反応条件

温度
100 °C

実験手順

6-(3-ethylureido)-4-(4-(trifluoromethyl)thiazol-2-yl)pyridin-3-ylboronic acid (Intermediate 9, 0.350 g, 0.97 mmol) and (S)-ethyl 6-bromo-1-(1-(2-morpholinoethyl)piperidin-3-yl)-4-oxo-1,4-dihydro-1,8-naphthyridine-3-carboxylate (Intermediate 34, 0.480 g, 0.97 mmol) were taken up in dioxane (4 mL), Cs2CO3 (0.633 g, 1.94 mmol) in water (1.000 mL) was added followed by Pd(PPh3)4 (0.112 g, 0.10 mmol). The reaction mixture was heated to 100° C. for 2 h, then 2 ml of 2N LiOH were added and stirred at 100° C. for an additional 30 min. The reaction mixture was cooled to room temperature and solvent evaporated. The resulting residue was taken back up in DMSO (2 ml) and filtered. DMSO solution was purified on an ISCO C18 column using water and acetonitrile. (S)-6-(6-(3-ethylureido)-4-(4-(trifluoromethyl)thiazol-2-yl)pyridin-3-yl)-1-(1-(2-morpholinoethyl)piperidin-3-yl)-4-oxo-1,4-dihydro-1,8-naphthyridine-3-carboxylic acid (0.080 g, 12%) is recovered as a pale yellow solid.

後処理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. customsolvent evaporated
  3. filtrationfiltered
  4. customDMSO solution was purified on an ISCO C18 column
  5. custom(S)-6-(6-(3-ethylureido)-4-(4-(trifluoromethyl)thiazol-2-yl)pyridin-3-yl)-1-(1-(2-morpholinoethyl)piperidin-3-yl)-4-oxo-1,4-dihydro-1,8-naphthyridine-3-carboxylic acid (0.080 g, 12%) is recovered as a pale yellow solid

出典と根拠

ORDレコード
ord-063d826c11c647ba9df14757fa08344c
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08569484B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート