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Water → HCID 14552387, 화합물

HRID 1761682
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HRID 1761682 반응식
[NH2:1][C@@H:2]1[CH2:11][CH2:10][C:5]2([O:9][CH2:8][CH2:7][O:6]2)[CH2:4][C@H:3]1[C:12]([O:14][CH2:15][CH3:16])=[O:13].C(=O)([O-])[O-].[K+].[K+].[CH2:23](Br)[CH2:24][CH3:25].O>CN(C=O)C>[CH2:23]([NH:1][C@@H:2]1[CH2:11][CH2:10][C:5]2([O:9][CH2:8][CH2:7][O:6]2)[CH2:4][C@H:3]1[C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH2:24][CH3:25]
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참가 물질

6

반응물 4

HCID 962WaterHCID 78401-BromopropaneHCID 11430Potassium CarbonateHCID 14552385HCID 14552385, 화합물

생성물 1

HCID 14552387HCID 14552387, 화합물수율 96.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
50 °C

실험 절차

Ethyl 8-amino-trans-1,4-dioxaspiro[4.5]decane-7-carboxylate (118.0 g, 0.52 mole) was dissolved in DMF (1 l) and potassium carbonate (107 g, 0.77 mole) and propyl bromide (158.4 g, 1.3 mole) were added. The mixture was heated to 50° C. for three hours, then poured into water, and the hydrogen ion concentration was adjusted to pH 10. The product was extracted with methylene chloride, dried and evaporated to give 136 g of a dark orange oil.

후처리

  1. concentrationthe hydrogen ion concentration
  2. extractionThe product was extracted with methylene chloride
  3. customdried
  4. customevaporated

출처 및 근거

ORD 기록
ord-44b16510fc4a46f58f95c76a3e9cf4a1
출처 데이터셋
uspto-grants-1989_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04826986

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