1,4-Dioxane hydrochloride → HCID 21137721、化合物

HRID 1358581ノート

反応式

HRID 1358581 の反応式
[CH3:1][O:2][C:3](=[O:30])[C@H:4]([CH3:29])[NH:5][C:6]1[CH:11]=[CH:10][C:9]([O:12][CH2:13][C:14]([O:16]C(C)(C)C)=[O:15])=[CH:8][C:7]=1[C:21](=[O:28])[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1.Cl.O1CCOCC1>O1CCOCC1>[CH3:1][O:2][C:3](=[O:30])[C@H:4]([CH3:29])[NH:5][C:6]1[CH:11]=[CH:10][C:9]([O:12][CH2:13][C:14]([OH:16])=[O:15])=[CH:8][C:7]=1[C:21](=[O:28])[C:22]1[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=1

参加物

4

反応物 2

HCID 204431481,4-Dioxane hydrochlorideHCID 21137722HCID 21137722、化合物

生成物 1

HCID 21137721HCID 21137721、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A mixture of 4-t-butoxycarbonylmethoxy-N-(2-benzoylphenyl)alanine methyl ester (1.4 g), 4N hydrogen chloride/dioxane (10 ml) and dioxane (10 ml) was stirred at room temperature for 3 hours and allowed to stand overnight. The reaction mixture was concentrated under reduced pressure. To the residue was added toluene and the mixture was concentrated under reduced pressure. The residue was chromatographed on a silica gel column (LiChroprepDIOL (Merck)) using hexane: ethyl acetate=2:1−1:1 as the eluant to afford the title compound (0.87 g, Rf=0.53: thin layer chromatography on a silica gel plate using hexane: ethyl acetate=3:2 as the eluant).

後処理

  1. waitto stand overnight
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. additionTo the residue was added toluene
  4. concentrationthe mixture was concentrated under reduced pressure
  5. customThe residue was chromatographed on a silica gel column (LiChroprepDIOL (Merck))

出典と根拠

ORDレコード
ord-09c6ccdd961e4b6d9517a89f30f242e2
出典データセット
uspto-grants-2003_07
特許番号
US06596751B2

反応ノート

読み込み中…