Triethylamine → N,N'-Bis(benzyloxycarbonyl)-3-[carboxymethoxyacetyl]-3-azapentane-1,5-diamine

HRID 1067175

反応式

HRID 1067175 の反応式
[CH2:1]([O:8][C:9]([NH:11][CH2:12][CH2:13][NH:14][CH2:15][CH2:16][NH:17][C:18]([O:20][CH2:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)=[O:19])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:28]1(=[O:35])[O:34][C:32](=[O:33])[CH2:31][O:30][CH2:29]1.C(N(CC)CC)C>CN(C=O)C>[CH2:1]([O:8][C:9]([NH:11][CH2:12][CH2:13][N:14]([C:32](=[O:33])[CH2:31][O:30][CH2:29][C:28]([OH:35])=[O:34])[CH2:15][CH2:16][NH:17][C:18]([O:20][CH2:21][C:22]1[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=1)=[O:19])=[O:10])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 782321,4-Dioxane-2,6-dioneHCID 4367374N,N''-Di-Z-diethylenetriamine

生成物 1

HCID 54008985N,N'-Bis(benzyloxycarbonyl)-3-[carboxymethoxyacetyl]-3-azapentane-1,5-diamine

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

37.14 g (100 mmol) of the bis(benzyloxycarbonylaminoethyl)-amine described in Example 1a is dissolved in DMF, mixed in an ice bath with 17.4 g (150 mmol) of diglycolic anhydride (Janssen Chimica) and 21 ml (150 mmol) of triethylamine and then stirred overnight at room temperature. The solution is concentrated by evaporation in a vacuum, the residue is taken up in ethyl acetate and shaken out with diluted hydrochloric acid. The organic phase is dried with sodium sulfate and after filtration from drying agent, it is crystallized by adding hexane.

後処理

  1. concentrationThe solution is concentrated by evaporation in a vacuum
  2. stirringshaken out with diluted hydrochloric acid
  3. dry with materialThe organic phase is dried with sodium sulfate
  4. filtrationafter filtration
  5. customfrom drying agent, it
  6. customis crystallized
  7. additionby adding hexane

出典と根拠

ORDレコード
ord-47f7d99797424acb961b5b03aec76798
出典データセット
uspto-grants-2001_06
特許番号
US06248306B1

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