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Dimethylamine → 4-Benzyloxy-1-dimethylaminocyclohexanecarbonitrile

HRID 1349382
ノート
印刷プレビュー

反応式

HRID 1349382 の反応式
[CH3:1][NH:2][CH3:3].[CH2:4]([O:11][CH:12]1[CH2:17][CH2:16][C:15](=O)[CH2:14][CH2:13]1)[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.Cl.[CH3:20][NH:21]C.[C-]#N.[K+]>CO>[CH2:4]([O:11][CH:12]1[CH2:17][CH2:16][C:15]([N:2]([CH3:3])[CH3:1])([C:20]#[N:21])[CH2:14][CH2:13]1)[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 674DimethylamineHCID 9032Potassium CyanideHCID 10473Dimethylamine, hydrochlorideHCID 109873694-(Benzyloxy)cyclohexanone

生成物 1

HCID 210932404-Benzyloxy-1-dimethylaminocyclohexanecarbonitrile

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of 130 ml of 7.9 molar aqueous dimethylamine solution, 16 ml of methanol, 20.0 g of 4-benzyloxycyclohexanone, 23.2 g of dimethylamine hydrochloride and 15.3 g of potassium cyanide was stirred for 65 hours at room temperature; extraction was carried out four times using 120 ml of diethyl ether each time, and the combined extracts were concentrated; 100 ml of dichloromethane were added to the residue, the phases were separated, and the organic phases were dried over sodium sulfate, filtered and concentrated. 24.5 g of 4-benzyloxy-1-dimethylaminocyclohexanecarbonitrile were obtained in the form of a yellowish oil which slowly solidified.

後処理

  1. extractionextraction
  2. concentrationthe combined extracts were concentrated
  3. addition100 ml of dichloromethane were added to the residue
  4. customthe phases were separated
  5. dry with materialthe organic phases were dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-4c61180a1d2c49dba50468e13509358b
出典データセット
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07211694B2

反応ノート

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