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

HRID 1525853ノート

反応式

HRID 1525853 の反応式
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

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 69083351HCID 69083351、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒2 回

実験手順

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]+.

後処理

  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

出典と根拠

ORDレコード
ord-17f6540727ff438496b2f0e83f98c8a1
出典データセット
uspto-grants-2015_07
特許番号
US09084794B2

反応ノート

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