Hydrochloric Acid → HCID 71143553、化合物

HRID 2363287ノート

反応式

HRID 2363287 の反応式
O.[OH-].[Li+].[C:4]([CH2:6][C:7]1([N:22]2[CH:26]=[C:25]([C:27]3[C:28]4[CH:35]=[CH:34][N:33]([CH2:36][O:37][CH2:38][CH2:39][Si:40]([CH3:43])([CH3:42])[CH3:41])[C:29]=4[N:30]=[CH:31][N:32]=3)[CH:24]=[N:23]2)[CH2:10][N:9]([C:11]2[CH:20]=[CH:19][C:14]([C:15]([O:17]C)=[O:16])=[CH:13][C:12]=2[F:21])[CH2:8]1)#[N:5].Cl>CO.O>[C:4]([CH2:6][C:7]1([N:22]2[CH:26]=[C:25]([C:27]3[C:28]4[CH:35]=[CH:34][N:33]([CH2:36][O:37][CH2:38][CH2:39][Si:40]([CH3:41])([CH3:43])[CH3:42])[C:29]=4[N:30]=[CH:31][N:32]=3)[CH:24]=[N:23]2)[CH2:8][N:9]([C:11]2[CH:20]=[CH:19][C:14]([C:15]([OH:17])=[O:16])=[CH:13][C:12]=2[F:21])[CH2:10]1)#[N:5]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 168937Lithium hydroxide, monohydrateHCID 71143540HCID 71143540、化合物

生成物 1

HCID 71143553HCID 71143553、化合物収率 91.9%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

反応条件

温度
40 °C

実験手順

Lithium hydroxide monohydrate (0.21 g, 5.0 mmol) was added to a mixture of methyl 4-{3-(cyanomethyl)-3-[4-(7-{[2-(trimethylsilyl)ethoxy]methyl}-7H-pyrrolo[2,3-d]pyrimidin-4-yl)-1H-pyrazol-1-yl]azetidin-1-yl}-3-fluorobenzoate (1.06 g) in methanol (15.0 mL) and water (3.0 mL). The reaction mixture was stirred at 40° C. overnight. The mixture was adjusted to pH 3 with aqueous HCl (1.00 N), and concentrated under reduced pressure to remove methanol. The solid formed was filtered and washed with water, and dried under reduced pressure to afford the crude product (0.95 g) which was directly used in next step reaction without further purification. LCMS (M+H)+: m/z=548.3.

後処理

  1. concentrationconcentrated under reduced pressure
  2. customto remove methanol
  3. customThe solid formed
  4. filtrationwas filtered
  5. washwashed with water
  6. customdried under reduced pressure

出典と根拠

ORDレコード
ord-de55210c25b444f1b7f79049dde54b5f
出典データセット
uspto-grants-2014_04
特許番号
US08691807B2

反応ノート

読み込み中…