Sodium Hydroxide → 4-Cyclopropyl-1-oxa-4,9-diazaspiro[5.5]undecan-3-one

HRID 1525853노트

반응식

HRID 1525853 반응식
Cl.[CH:2]1([N:5]2[CH2:10][C:9]3([CH2:15][CH2:14][NH:13][CH2:12][CH2:11]3)[O:8][CH2:7][C:6]2=[O:16])[CH2:4][CH2:3]1.[OH-].[Na+]>ClCCl.O>[CH:2]1([N:5]2[CH2:10][C:9]3([CH2:11][CH2:12][NH:13][CH2:14][CH2:15]3)[O:8][CH2:7][C:6]2=[O:16])[CH2:4][CH2:3]1

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 69083351HCID 69083351, 화합물

생성물 1

HCID 667837534-Cyclopropyl-1-oxa-4,9-diazaspiro[5.5]undecan-3-one수율 80%

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매2회

실험 절차

A suspension of 4-cyclopropyl-1-oxa-4,9-diazaspiro[5.5]undecan-3-one hydrochloride (8.11 mmol) in dichloromethane (10 mL) was treated with 1N aq NaOH (10.00 mmol). The biphasic mixture was stirred for 1 hour, at which point the cloudy organic layer had turned clear. The contents of the flask were further diluted with water (50 mL) and dichloromethane (50 mL) and the layers were separated. The aqueous layer was extracted with dichloromethane. The organic layers were combined, dried over sodium sulfate, filtered and concentrated in vacuo to afford the title compound as a yellow oil (80%). MS(ES)+ m/e 211.2 [M+H]+.

후처리

  1. customthe layers were separated
  2. extractionThe aqueous layer was extracted with dichloromethane
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-17f6540727ff438496b2f0e83f98c8a1
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09084794B2

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