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Hydrochloric Acid → HCID 70175216、化合物

HRID 2186347
ノート
印刷プレビュー

反応式

HRID 2186347 の反応式
[OH-].[Na+].[CH3:3][O:4][C:5]1[CH:6]=[C:7]2[C:12](=[CH:13][CH:14]=1)[N:11]=[CH:10][CH:9]=[C:8]2[CH2:15][CH2:16][CH2:17][C@@H:18]1[CH2:23][CH2:22][N:21]([CH2:24][CH2:25][S:26][C:27]2[S:28][CH:29]=[CH:30][CH:31]=2)[CH2:20][C@@H:19]1[C:32]([O:34]C)=[O:33].[ClH:36]>CO.O.ClCCl.CO>[ClH:36].[ClH:36].[CH3:3][O:4][C:5]1[CH:6]=[C:7]2[C:12](=[CH:13][CH:14]=1)[N:11]=[CH:10][CH:9]=[C:8]2[CH2:15][CH2:16][CH2:17][C@@H:18]1[CH2:23][CH2:22][N:21]([CH2:24][CH2:25][S:26][C:27]2[S:28][CH:29]=[CH:30][CH:31]=2)[CH2:20][C@@H:19]1[C:32]([OH:34])=[O:33]
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

7

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 86758151HCID 86758151、化合物

生成物 1

HCID 70175216HCID 70175216、化合物

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒
HCID 21226129
Dichloromethane methanol
溶媒

反応条件

温度
60 °C

実験手順

0.5 cm3 of 5N aqueous sodium hydroxide was added to a stirred solution of 0.34 g of methyl (3R,4R)-4-[3-(6-methoxyquinolin-4-yl)propyl]-1-[2-(thien-2-ylthio)ethyl]piperidine-3-carboxylate in 3 cm3 of methanol and then the mixture was heated at a temperature in the region of 60° C. for 20 hours. After evaporating the solvents under reduced pressure (5 kPa) at a temperature in the region of 40° C., the residue obtained was taken up in 5 cm3 of water and then acidified by addition of 1 cm3 of 35% hydrochloric acid. The mixture was again evaporated under reduced pressure under the same conditions as above; the residue obtained was taken up in 5 cm3 of a dichloromethane/methanol (90/10 by volume) mixture. The insoluble material was filtered off and then the solvent was evaporated under reduced pressure (5 kPa) at a temperature in the region of 40° C. 0.35 g of (3R,4R)-4-[3-(6-methoxyquinolin-4-yl)propyl]-1-[2-(thien-2-ylthio)ethyl]piperidine-3-carboxylic acid dihydrochloride was obtained in the form of a solid with a beige color which melts with softening in the region of 150° C.

後処理

  1. customAfter evaporating the solvents under reduced pressure (5 kPa) at a temperature in the region of 40° C.
  2. customthe residue obtained
  3. customThe mixture was again evaporated under reduced pressure under the same conditions as above
  4. customthe residue obtained
  5. filtrationThe insoluble material was filtered off
  6. customthe solvent was evaporated under reduced pressure (5 kPa) at a temperature in the region of 40° C

出典と根拠

ORDレコード
ord-4cb9062afb35435aa589966af6b91900
出典データセット
uspto-grants-2002_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06403610B1

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