Hydrochloric Acid → 10-[2-[(3-Carboxy-2,4,6-triiodophenyl)amino]-2-oxoethyl]-1,4,7,10-tetraazacyclododecane-1,4,7-triacetic acid

HRID 2258394ノート

反応式

HRID 2258394 の反応式
Br[CH2:2][C:3]([OH:5])=[O:4].[C:6]([C:9]1[C:10]([I:33])=[C:11]([NH:17][C:18](=[O:32])[CH2:19][N:20]2[CH2:31][CH2:30][NH:29][CH2:28][CH2:27][NH:26][CH2:25][CH2:24][NH:23][CH2:22][CH2:21]2)[C:12]([I:16])=[CH:13][C:14]=1[I:15])([OH:8])=[O:7].Cl>O.[OH-].[Na+]>[C:6]([C:9]1[C:10]([I:33])=[C:11]([NH:17][C:18](=[O:32])[CH2:19][N:20]2[CH2:31][CH2:30][N:29]([CH2:2][C:3]([OH:5])=[O:4])[CH2:28][CH2:27][N:26]([CH2:2][C:3]([OH:5])=[O:4])[CH2:25][CH2:24][N:23]([CH2:2][C:3]([OH:5])=[O:4])[CH2:22][CH2:21]2)[C:12]([I:16])=[CH:13][C:14]=1[I:15])([OH:8])=[O:7]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 6227Bromoacetic AcidHCID 22921403N-(3-carboxy-2,4,6-triiodophenyl)-1,4,7,10-tetraazacyclododecane-1-acetamide

生成物 1

HCID 1074891610-[2-[(3-Carboxy-2,4,6-triiodophenyl)amino]-2-oxoethyl]-1,4,7,10-tetraazacyclododecane-1,4,7-triacetic acid収率 71%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 14798Sodium Hydroxide溶媒3 回

実験手順

18.9 g of bromoacetic acid (product available on the market) (0.136 mol) are dissolved in 20 ml of H2O, and by keeping the temperature below 10° C., the solution pH is adjusted to 5 with 68 ml of 2N NaOH (0.136 mol). After adding a solution of 30 g of compound. (B) N-(3-carboxy-2,4,6-triiodophenyl)-1,4,7,10-tetraazacyclododecane-1-acetamide (0.041 mol) in 20.5 ml of 2N NaOH, the reaction mixture is heated at 50° C. for 15 h keeping the pH at 10 with 6.15 ml of 2N NaOH (0.123 mol). A solid precipitates which is then filtered and dissolved in 200 ml of H2O. After acidification of the solution with 82 ml of HCl 2N (0.164 mol) the precipitate is filtered. 28.2 g of 10-[2-[(3-carboxy-2,4,6-triiodophenyl)amino]-2-oxoethyl]-1,4,7,10-tetraazacyclododecane-1,4,7-triacetic acid (0.029 mol) are obtained.

後処理

  1. customthe temperature below 10° C.
  2. customA solid precipitates which
  3. filtrationis then filtered
  4. dissolutiondissolved in 200 ml of H2O

出典と根拠

ORDレコード
ord-d2da61e57cc64d90bc62943fe6628b6c
出典データセット
uspto-grants-1997_08
特許番号
US05660814

反応ノート

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