1,1'-Dimethyl 2,2'-oxybis(acetate) → 5,9-Bis(benzyloxymethyl)-1-oxa-4,7,10-triazacyclododecane-3,11-dione

HRID 1614520

反応式

HRID 1614520 の反応式
[NH2:1][CH:2]([CH2:17][O:18][CH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[CH2:3][NH:4][CH2:5][CH:6]([NH2:16])[CH2:7][O:8][CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.C[O:27][C:28](=O)[CH2:29][O:30][CH2:31][C:32](OC)=[O:33]>CO>[CH2:19]([O:18][CH2:17][CH:2]1[CH2:3][NH:4][CH2:5][CH:6]([CH2:7][O:8][CH2:9][C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=2)[NH:16][C:32](=[O:33])[CH2:31][O:30][CH2:29][C:28](=[O:27])[NH:1]1)[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1

参加物

4

反応物 2

HCID 2018771,1'-Dimethyl 2,2'-oxybis(acetate)HCID 194385191,5-Diamino-1,5-dibenzyloxymethyl-3-azapentane

生成物 1

HCID 194385105,9-Bis(benzyloxymethyl)-1-oxa-4,7,10-triazacyclododecane-3,11-dione

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

1,5-Diamino-1,5-dibenzyloxymethyl-3-aza-pentane (0.250 g, 0.73 mmol) (Example 6 (d)) and diglycolic acid dimethyl ester (0.118 g, 0.73 mmol) were dissolved in methanol (20 ml). The mixture was refluxed for 6 days. The solvent was evaporated and the mixture chromatographed on a silica column. 5,9-Bis(benzyloxymethyl)-1-oxa-4,7,10-triazacyclododecane -3,11-dione was isolated as a yellow oil. Yield 0.273 g (85%). FAB MS: 442(M+1).

後処理

  1. temperatureThe mixture was refluxed for 6 days
  2. customThe solvent was evaporated
  3. customthe mixture chromatographed on a silica column

出典と根拠

ORDレコード
ord-00f9d8ec1268454f8bf1ce31e3dcf480
出典データセット
uspto-grants-1993_03
特許番号
US05198208

関連ノート

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