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Hydrochloric Acid → HCID 69202507、化合物

HRID 2220599
ノート
印刷プレビュー

反応式

HRID 2220599 の反応式
[OH-].[Na+].[CH2:3]([O:10][C:11]1[CH:16]=[CH:15][C:14]([C@@H:17]([OH:27])[C@@H:18]([NH:20]C(=O)C(F)(F)F)[CH3:19])=[CH:13][C:12]=1[NH:28][S:29]([CH3:32])(=[O:31])=[O:30])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.Cl>CO>[NH2:20][C@@H:18]([CH3:19])[C@@H:17]([C:14]1[CH:15]=[CH:16][C:11]([O:10][CH2:3][C:4]2[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=2)=[C:12]([NH:28][S:29]([CH3:32])(=[O:31])=[O:30])[CH:13]=1)[OH:27]
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 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 86611768N-[(1S,2R)-2-(4-Benzyloxy-3-methanesulfonylaminophenyl)-2-hydroxy-1-methylethyl]-2,2,2-trifluoroacetamide

生成物 1

HCID 69202507HCID 69202507、化合物収率 810.7%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A 5 mol/L aqueous solution of sodium hydroxide (6.3 mL) was added to a solution of N-[(1S,2R)-2-(4-benzyloxy-3-methanesulfonylaminophenyl)-2-hydroxy-1-methylethyl]-2,2,2-trifluoroacetamide (5.5 g) in methanol (100 mL) at room temperature, and the mixture was heated under reflux for 5.5 hrs. After being cooled to room temperature, 2 mol/L hydrochloric acid (15.7 mL) was added to the mixture. The solvent was evaporated under reduced pressure, and the residue was purified by aminopropyl silica gel column chromatography (eluent: ethanol) to afford the title compound (35 g).

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 5.5 hrs
  3. customThe solvent was evaporated under reduced pressure
  4. customthe residue was purified by aminopropyl silica gel column chromatography (eluent: ethanol)

出典と根拠

ORDレコード
ord-2ccc791abe674e1ab3b4f089243339bb
出典データセット
uspto-grants-2008_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07417169B2

反応ノート

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