1,4-Dioxane-2,6-dione → HCID 86619729、化合物

HRID 254689ノート

反応式

HRID 254689 の反応式
[N:1]([CH2:4][CH2:5][O:6][CH2:7][CH2:8][O:9][CH2:10][CH2:11][O:12][CH2:13][CH2:14][O:15][CH2:16][CH2:17][O:18][CH2:19][CH2:20][NH2:21])=[N+:2]=[N-:3].[C:22]1(=[O:29])[O:28][C:26](=[O:27])[CH2:25][O:24][CH2:23]1>ClCCl.O>[N:1]([CH2:4][CH2:5][O:6][CH2:7][CH2:8][O:9][CH2:10][CH2:11][O:12][CH2:13][CH2:14][O:15][CH2:16][CH2:17][O:18][CH2:19][CH2:20][NH:21][C:26](=[O:27])[CH2:25][O:24][CH2:23][C:22]([OH:29])=[O:28])=[N+:2]=[N-:3]

参加物

5

反応物 2

HCID 782321,4-Dioxane-2,6-dioneHCID 2189447617-Azido-3,6,9,12,15-pentaoxaheptadecan-1-amine

生成物 1

HCID 86619729HCID 86619729、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 17-azido-3,6,9,12,15-pentaoxaheptadecanamine (15 g, 50 mmol) in dichloromethane (100 mL) was added diglycolic anhydride (Acros, 6.4 g, 55 mmol). The reaction mixture was stirred overnight. The reaction was monitored by ESI-MS analysis, and more reagents were added to drive the reaction to completion. The solution was concentrated to give a yellow residue which was dissolved in water (250 mL). The product was isolated from the aqueous phase by continuous extraction with dichloromethane over night. Drying and evaporation of the solvent gave a yield of 18 g (85%). The product was characterized by ESI-MS analysis (MH+ calculated: 423.20; found 423.4). The product was used in the next step without further purification.

後処理

  1. additionwere added
  2. customthe reaction to completion
  3. concentrationThe solution was concentrated
  4. customto give a yellow residue which
  5. customDrying
  6. customevaporation of the solvent
  7. customgave a yield of 18 g (85%)
  8. customThe product was used in the next step without further purification

出典と根拠

ORDレコード
ord-0f9774b2c208400080d77ef1dad759b3
出典データセット
uspto-grants-2011_01
特許番号
US07875701B2

反応ノート

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