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Diethyl Ether → 2,4,6-Triiodo-1,3,5-tris-(aminoethoxymethyl)benzene

HRID 1271813
ノート
印刷プレビュー

反応式

HRID 1271813 の反応式
[I:1][C:2]1[C:7]([CH2:8][O:9][CH2:10][CH2:11][NH:12]C(OC(C)(C)C)=O)=[C:6]([I:20])[C:5]([CH2:21][O:22][CH2:23][CH2:24][NH:25]C(OC(C)(C)C)=O)=[C:4]([I:33])[C:3]=1[CH2:34][O:35][CH2:36][CH2:37][NH:38]C(OC(C)(C)C)=O.FC(F)(F)C(O)=O.C(OCC)C.[OH-].[Na+]>ClCCl.O>[I:1][C:2]1[C:3]([CH2:34][O:35][CH2:36][CH2:37][NH2:38])=[C:4]([I:33])[C:5]([CH2:21][O:22][CH2:23][CH2:24][NH2:25])=[C:6]([I:20])[C:7]=1[CH2:8][O:9][CH2:10][CH2:11][NH2:12]
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 4

HCID 3283Diethyl Ether2 回HCID 6422Trifluoroacetic acidHCID 14798Sodium HydroxideHCID 184548882,4,6-Triiodo-1,3,5-tris-(2-tert-butoxycarbonylaminoethoxymethyl)benzene

生成物 1

HCID 865956492,4,6-Triiodo-1,3,5-tris-(aminoethoxymethyl)benzene

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

24.4 g (25 mmol) of 2,4,6-triiodo-1,3,5-tris-(2-tert-butoxycarbonylaminoethoxymethyl)benzene is dissolved in 100 ml of dichloromethane, mixed at 0° C. with 100 ml of trifluoroacetic acid and stirred for 3 hours at 0° C. The batch is poured into 500 ml of diethyl ether, the solid that accumulates in this case is suctioned off and rewashed several times with diethyl ether. The residue is dissolved in 100 ml of water and 100 ml of dichloromethane while being stirred vigorously, and 32% NaOH solution is added until a pH of 10 is reached. The organic phase is separated, the aqueous phase is extracted three times with 50 ml each of dichloromethane, the combined organic phases are dried on magnesium sulfate and evaporated to the dry state.

後処理

  1. customThe organic phase is separated
  2. extractionthe aqueous phase is extracted three times with 50 ml each of dichloromethane
  3. customthe combined organic phases are dried on magnesium sulfate
  4. customevaporated to the dry state

出典と根拠

ORDレコード
ord-2a0584e5107a4ab896d189fb059aa205
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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