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Water → 2,4,6-Triiodo-1,3,5-tris-(2-tert-butoxycarbonylaminoethoxymethyl)benzene

HRID 1271812
ノート
印刷プレビュー

反応式

HRID 1271812 の反応式
[C:1]([O:5][C:6]([NH:8][CH2:9][CH2:10]OS(C1C(C)=CC=CC=1)(=O)=O)=[O:7])([CH3:4])([CH3:3])[CH3:2].[I:22][C:23]1[C:28]([CH2:29][OH:30])=[C:27]([I:31])[C:26]([CH2:32][OH:33])=[C:25]([I:34])[C:24]=1[CH2:35][OH:36].[OH2:37]>C1(C)C=CC=CC=1.S([O-])(O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC.[OH-].[Na+]>[I:22][C:23]1[C:24]([CH2:35][O:36][CH2:10][CH2:9][NH:8][C:6]([O:5][C:1]([CH3:4])([CH3:3])[CH3:2])=[O:37])=[C:25]([I:34])[C:26]([CH2:32][O:33][CH2:10][CH2:9][NH:8][C:6]([O:5][C:1]([CH3:4])([CH3:3])[CH3:2])=[O:7])=[C:27]([I:31])[C:28]=1[CH2:29][O:30][CH2:10][CH2:9][NH:8][C:6]([O:5][C:1]([CH3:2])([CH3:3])[CH3:4])=[O:7]
参加物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 962WaterHCID 206936271,3,5-Triiodo-2,4,6-trihydroxymethylbenzeneHCID 86595648Toluenesulfonic acid-2-tert-butoxycarbonylaminoethyl ester

生成物 1

HCID 184548882,4,6-Triiodo-1,3,5-tris-(2-tert-butoxycarbonylaminoethoxymethyl)benzene

試薬・触媒・溶媒 3

HCID 94433Tetrabutylammonium hydrogen sulfate触媒
HCID 1140
Toluene
溶媒
2 回
HCID 14798Sodium Hydroxide溶媒

実験手順

142 g (450 mmol) of toluenesulfonic acid-2-tert-butoxycarbonylaminoethyl ester (Canne et al., Tetrahedron Letters, 38, 1997, 3361), dissolved in 250 ml of toluene, is added in drops to a mixture that consists of 50.0 g (91.4 mmol) of 1,3,5-triiodo-2,4,6-trishydroxymethylbenzene, and 3 g (8.7 mmol) of tetrabutylammonium hydrogen sulfate in 200 ml of 32% NaOH solution and 300 ml of toluene at room temperature, and then it is stirred for 12 hours. It is mixed with water and extracted twice with 300 ml each of toluene. The combined organic phases are dried on sodium sulfate, the solvent is evaporated to the dry state and chromatographed on silica gel (mobile solvent:hexane/ethyl acetate 10:1). The fractions that contain the product are combined and concentrated by evaporation.

後処理

  1. additionis added in drops to a mixture that
  2. extractionextracted twice with 300 ml each of toluene
  3. customThe combined organic phases are dried on sodium sulfate
  4. customthe solvent is evaporated to the dry state
  5. customchromatographed on silica gel (mobile solvent:hexane/ethyl acetate 10:1)
  6. concentrationconcentrated by evaporation

出典と根拠

ORDレコード
ord-9abac11493ac4164ab4a1c87ab3570b7
出典データセット
uspto-grants-2007_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07208140B2

反応ノート

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