Sodium Hydroxide → HCID 18454886、化合物

HRID 1271805ノート

反応式

HRID 1271805 の反応式
[CH2:1]([O:8][C:9]([N:11]1[CH2:22][CH2:21][N:20]([CH2:23][C:24]([O:26]CC)=[O:25])[CH2:19][CH2:18][N:17]([C:29]([O:31][CH2:32][C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)=[O:30])[CH2:16][CH2:15][N:14]([C:39]([O:41][CH2:42][C:43]2[CH:48]=[CH:47][CH:46]=[CH:45][CH:44]=2)=[O:40])[CH2:13][CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[Na+]>O1CCOCC1>[CH2:1]([O:8][C:9]([N:11]1[CH2:22][CH2:21][N:20]([CH2:23][C:24]([OH:26])=[O:25])[CH2:19][CH2:18][N:17]([C:29]([O:31][CH2:32][C:33]2[CH:34]=[CH:35][CH:36]=[CH:37][CH:38]=2)=[O:30])[CH2:16][CH2:15][N:14]([C:39]([O:41][CH2:42][C:43]2[CH:48]=[CH:47][CH:46]=[CH:45][CH:44]=2)=[O:40])[CH2:13][CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 184548871,4,7-Tris-(benzyloxycarbonyl)-10-(ethoxycarbonylmethyl)-1,4,7,10-tetrazacyclododecane

生成物 1

HCID 18454886HCID 18454886、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

34 g (51.4 mmol) of 1,4,7-tris-(benzyloxycarbonyl)-10-(ethoxycarbonylmethyl)-1,4,7,10-tetrazacyclododecane is dissolved in 300 ml of dioxane and mixed with 144 ml of 5% aqueous NaOH solution and stirred for 24 hours at room temperature. After neutralization with concentrated HCl, it is evaporated to the dry state. The residue is taken up in 250 ml of ethyl acetate and extracted twice with 250 ml each of 1N HCl solution. The organic phase is dried on sodium sulfate, and the solvent is evaporated to the dry state.

後処理

  1. customAfter neutralization with concentrated HCl, it is evaporated to the dry state
  2. extractionextracted twice with 250 ml each of 1N HCl solution
  3. customThe organic phase is dried on sodium sulfate
  4. customthe solvent is evaporated to the dry state

出典と根拠

ORDレコード
ord-233b802a1dcd4c22822cb4dc157b6512
出典データセット
uspto-grants-2007_04
特許番号
US07208140B2

反応ノート

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