1,4-Dioxane-2,6-dione → HCID 86619729, 화합물

HRID 709336노트

반응식

HRID 709336 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

HCID 86619729HCID 86619729, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매2회

실험 절차

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 overnight. 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.

후처리

  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

출처 및 근거

ORD 기록
ord-4321f58755c140b0a4ded1978689a658
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09180213B2

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