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Water → HCID 71656972、化合物

HRID 632589
ノート
印刷プレビュー

反応式

HRID 632589 の反応式
[F:1][C:2]1([F:52])[CH2:7][CH2:6][CH:5]([C:8]2[C:17]3[C@@H:16]([OH:18])[CH2:15][C:14]([CH3:20])([CH3:19])[CH2:13][C:12]=3[N:11]=[C:10]([CH:21]3[CH2:26][CH2:25][N:24]([C:27]4[N:32]=[CH:31][C:30]([O:33][CH2:34][CH2:35][C:36]([OH:39])([CH3:38])[CH3:37])=[CH:29][N:28]=4)[CH2:23][CH2:22]3)[C:9]=2[C@@H:40]([F:51])[C:41]2[CH:46]=[CH:45][C:44]([C:47]([F:50])([F:49])[F:48])=[CH:43][CH:42]=2)[CH2:4][CH2:3]1.[C:53]([OH:60])(=[O:59])[CH2:54][CH2:55][C:56]([OH:58])=[O:57].O>CC(C)=O>[C:53]([OH:60])(=[O:59])[CH2:54][CH2:55][C:56]([OH:58])=[O:57].[C:53]([OH:60])(=[O:59])[CH2:54][CH2:55][C:56]([OH:58])=[O:57].[F:52][C:2]1([F:1])[CH2:3][CH2:4][CH:5]([C:8]2[C:17]3[C@@H:16]([OH:18])[CH2:15][C:14]([CH3:19])([CH3:20])[CH2:13][C:12]=3[N:11]=[C:10]([CH:21]3[CH2:22][CH2:23][N:24]([C:27]4[N:32]=[CH:31][C:30]([O:33][CH2:34][CH2:35][C:36]([OH:39])([CH3:37])[CH3:38])=[CH:29][N:28]=4)[CH2:25][CH2:26]3)[C:9]=2[C@@H:40]([F:51])[C:41]2[CH:46]=[CH:45][C:44]([C:47]([F:48])([F:50])[F:49])=[CH:43][CH:42]=2)[CH2:6][CH2:7]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 1110Succinic AcidHCID 71656881HCID 71656881、化合物

生成物 1

HCID 71656972HCID 71656972、化合物収率 39%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒2 回

実験手順

To 40.8 mg (0.056 mmol) of (5S)-4-(4,4-Difluorocyclohexyl)-3-{(S)-fluoro[4-(trifluoromethyl)phenyl]methyl}-2-{1-[5-(3-hydroxy-3-methylbutoxy)pyrimidin-2-yl]piperidin-4-yl}-7,7-dimethyl-5,6,7,8-tetrahydroquinolin-5-ol, which was prepared by a method similar to that of Reference Example 16, and 13.1 mg (0.11 mmol) of succinic acid, 0.08 ml of acetone and 0.008 ml of ultrapure water were added, and the reaction mixture was stirred at room temperature to obtain a homogeneous solution. A small amount of a seed crystal was added thereto, then 0.02 ml of acetone was added, and the reaction mixture was stirred for 30 minutes. The precipitated solid was obtained by filtration, washed with 0.4 ml of acetone and then dried under reduced pressure at 40° C. to provide 18.7 mg of the title compound as a white powder (yield: 39%).

後処理

  1. additionwere added
  2. customto obtain a homogeneous solution
  3. additionA small amount of a seed crystal was added
  4. stirringthe reaction mixture was stirred for 30 minutes
  5. customThe precipitated solid was obtained by filtration
  6. washwashed with 0.4 ml of acetone
  7. customdried under reduced pressure at 40° C.

出典と根拠

ORDレコード
ord-faacc259d8ee4ea6a2cb5a33200e5fe4
出典データセット
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09321747B2

反応ノート

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