Dimethyl Sulfoxide → (4-Benzylmorpholin-2-yl)(cyclopropyl)methanone

HRID 30323ノート

反応式

HRID 30323 の反応式
CS(C)=O.C(Cl)(=O)C(Cl)=O.[CH2:11]([N:18]1[CH2:23][CH2:22][O:21][CH:20]([CH:24]([CH:26]2[CH2:28][CH2:27]2)[OH:25])[CH2:19]1)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.C(N(CC)CC)C>C(Cl)Cl.O>[CH:26]1([C:24]([CH:20]2[O:21][CH2:22][CH2:23][N:18]([CH2:11][C:12]3[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=3)[CH2:19]2)=[O:25])[CH2:28][CH2:27]1

参加物

7

反応物 4

HCID 679Dimethyl SulfoxideHCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 59789293(4-Benzylmorpholin-2-yl)(cyclopropyl)methanol

生成物 1

HCID 59789271(4-Benzylmorpholin-2-yl)(cyclopropyl)methanone

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒3 回

実験手順

A solution of dimethylsulphoxide (0.69 mL, 9.7 mmol, 2.2 eq) in DCM (4.5 mL) is slowly added to a solution of oxalyl chloride (2.43 mL, 4.85 mmol, 1.1 eq) in DCM (2.5 mL) followed by a solution of 76 (1.09 g, 4.41 mmol) in DCM (0.7 mL) under nitrogen at −60° C. After stirring for 15 minutes, triethylamine (3.14 mL, 22.1 mmol, 5 eq) is added and stirring continues for 15 minutes. After addition of water, the layers are separated.

後処理

  1. stirringstirring
  2. waitcontinues for 15 minutes
  3. customthe layers are separated

出典と根拠

ORDレコード
ord-c4081059b5ec48d99cfec68090949e81
出典データセット
uspto-grants-2008_09
特許番号
US07423037B2

反応ノート

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