p-Toluenesulfonic acid monohydrate → HCID 58009754、化合物

HRID 494089ノート

反応式

HRID 494089 の反応式
[CH2:1]([O:8][C:9]([NH:11][CH2:12][C:13]([N:15]([CH2:17][CH:18](OC)OC)[CH3:16])=[O:14])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.C1(C)C=CC(S(O)(=O)=O)=CC=1>C1(C)C=CC=CC=1>[CH2:1]([O:8][C:9]([N:11]1[CH:18]=[CH:17][N:15]([CH3:16])[C:13](=[O:14])[CH2:12]1)=[O:10])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 58009747HCID 58009747、化合物

生成物 1

HCID 58009754HCID 58009754、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A solution of N2-benzyloxycarbonyl-N1-(2,2-dimethoxyethyl)-N1-methylglycinamide (1.9 Kg, 6.1 mol) and p-toluenesulfonic acid monohydrate (270 g) in toluene (29.4 L) was stirred at 80° C. for 4 hours. The resultant reaction mixture was cooled to room temperature, washed with water (4×2 L), dried over anhydrous magnesium sulfate, filtered, and concentrated under vacuum. The residual solid was subjected to column chromatography on silica gel eluting with heptane-ethyl acetate. Concentration of appropriate fractions provide the cyclization product as off-white solid.

後処理

  1. customThe resultant reaction mixture
  2. washwashed with water (4×2 L)
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-4f42d9375d184e05bda4b62d0cd44297
出典データセット
uspto-grants-2009_05
特許番号
US07538112B2

反応ノート

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