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Sodium Hydroxide → 3,5-Dichlorobenzyl 2-(2-((tert-butoxycarbonyl)amino)ethyl)morpholine-4-carboxylate

HRID 1480380
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HRID 1480380 반응식
[C:1]([O:5][C:6](=[O:16])[NH:7][CH2:8][CH2:9][CH:10]1[O:15][CH2:14][CH2:13][NH:12][CH2:11]1)([CH3:4])([CH3:3])[CH3:2].C(=O)(O)[O-].[Na+].[C:22](Cl)(=[O:33])[O:23][CH2:24][C:25]1[CH:30]=[C:29]([Cl:31])[CH:28]=[C:27]([Cl:32])[CH:26]=1.[OH-].[Na+]>C(Cl)Cl>[C:1]([O:5][C:6]([NH:7][CH2:8][CH2:9][CH:10]1[O:15][CH2:14][CH2:13][N:12]([C:22]([O:23][CH2:24][C:25]2[CH:26]=[C:27]([Cl:32])[CH:28]=[C:29]([Cl:31])[CH:30]=2)=[O:33])[CH2:11]1)=[O:16])([CH3:4])([CH3:2])[CH3:3]
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참가 물질

6

반응물 4

HCID 14798Sodium HydroxideHCID 516892Sodium BicarbonateHCID 133055323,5-Dichlorobenzyl ChloroformateHCID 25219056tert-Butyl (2-morpholin-2-ylethyl)carbamate

생성물 1

HCID 867226343,5-Dichlorobenzyl 2-(2-((tert-butoxycarbonyl)amino)ethyl)morpholine-4-carboxylate

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

실험 절차

To a mixture comprising of t-butyl(2-morpholin-2-ylethyl)carbamate (3 g, 13.03 mmol) in DCM (100 ml), was added saturated aqueous sodium bicarbonate solution (100 ml, 13.03 mmol), followed by 3,5-dichlorobenzyl carbonochloridate (3.43 g, 14.33 mmol). The biphasic mixture was stirred at room temperature for 2 hours. The resulting mixture was treated with 2M NaOH solution (50 ml). The reaction mixture was separated and the organic portion was dried over MgSO4 and concentrated under reduced pressure to afford the title compound.

후처리

  1. customThe reaction mixture was separated
  2. dry with materialthe organic portion was dried over MgSO4
  3. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-fda5ac0bfe854e7687b6dcfb80d6a62d
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09409895B2

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