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Acetone → HCID 70874615、化合物

HRID 2172277
ノート
印刷プレビュー

反応式

HRID 2172277 の反応式
C[O:2][C:3]1(OC)[CH2:8][CH2:7][N:6]([C:9]2[CH:28]=[CH:27][C:12]([O:13][CH2:14][C@@H:15]3[O:20][C:19]4=[N:21][C:22]([N+:24]([O-:26])=[O:25])=[CH:23][N:18]4[CH2:17][CH2:16]3)=[CH:11][CH:10]=2)[CH2:5][CH2:4]1.CC(C)=O.Cl>O>[N+:24]([C:22]1[N:21]=[C:19]2[N:18]([CH:23]=1)[CH2:17][CH2:16][C@H:15]([CH2:14][O:13][C:12]1[CH:11]=[CH:10][C:9]([N:6]3[CH2:5][CH2:4][C:3](=[O:2])[CH2:8][CH2:7]3)=[CH:28][CH:27]=1)[O:20]2)([O-:26])=[O:25]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 180AcetoneHCID 313Hydrochloric AcidHCID 86709411HCID 86709411、化合物

生成物 1

HCID 70874615HCID 70874615、化合物収率 99.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

(R)-7-[4-(4,4-Dimethoxypiperidin-1-yl)phenoxymethyl]-2-nitro-6,7-dihydro-5H-imidazo[2,1-b][1,3]oxazine (5.16 g), acetone (100 ml) and water (17 ml) were mixed. A 6 N hydrochloric acid aqueous solution (41 ml) was added thereto, followed by stirring at room temperature overnight. The reaction mixture was concentrated under reduced pressure. The remaining water layer was ice-cooled and neutralized by adding a 20% sodium carbonate aqueous solution. After being stirred at the same temperature for 10 minutes, the precipitated crystal was collected by filtration. The crystal thus obtained was dried at 60° C. to afford the title compound as a yellow solid (4.57 g).

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. temperaturecooled
  3. additionby adding a 20% sodium carbonate aqueous solution
  4. stirringAfter being stirred at the same temperature for 10 minutes
  5. filtrationthe precipitated crystal was collected by filtration
  6. customThe crystal thus obtained
  7. customwas dried at 60° C.

出典と根拠

ORDレコード
ord-d7cdb82536bf4bff9b339cd68cedcc42
出典データセット
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09051333B2

反応ノート

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