Diethylamine → HCID 45111295、化合物

HRID 1915989ノート

反応式

HRID 1915989 の反応式
[CH3:1][C:2]1([C:7]([OH:9])=O)[CH2:6][S:5][S:4][CH2:3]1.C(Cl)(=O)C(Cl)=O.[CH2:16]([NH:18][CH2:19][CH3:20])[CH3:17].C(N(C(C)C)CC)(C)C>ClCCl.CCCCCCC.CCOC(C)=O.CN(C=O)C>[CH2:16]([N:18]([CH2:19][CH3:20])[C:7]([C:2]1([CH3:1])[CH2:6][S:5][S:4][CH2:3]1)=[O:9])[CH3:17]

参加物

8

反応物 4

HCID 8021DiethylamineHCID 65578Oxalyl chlorideHCID 81531DiisopropylethylamineHCID 200693114-Methyl-1,2-dithiolane-4-carboxylic acid

生成物 1

HCID 45111295HCID 45111295、化合物

試薬・触媒・溶媒 3

HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane溶媒3 回HCID 21899848Ethylacetate heptane溶媒

反応条件

温度
0 °C

実験手順

5 ml of anhydrous dichloromethane and 0.1 ml of anhydrous DMF are added to 2.26 mmol of Compound 1. The mixture is cooled to 0° C. and 2.7 mmol of oxalyl chloride are added. The mixture is stirred at 20° C. and then added at 0° C. to a mixture of 2.26 mmol of diethylamine, 5 ml of anhydrous dichloromethane and 6.8 mmol of diisopropylethylamine. The reaction medium is stirred for 3 hours at 20° C. When the reaction is complete, the medium is diluted in 50 ml of dichloromethane and then washed with 2×30 ml of water and 1×50 ml of saturated NH4Cl solution, dried over Na2SO4 and evaporated to dryness on a rotavapor. After flash chromatography (eluent: heptane/EtOAc), Compound 18 is isolated in the form of a yellow oil (48% yield).

後処理

  1. stirringThe reaction medium is stirred for 3 hours at 20° C
  2. washwashed with 2×30 ml of water and 1×50 ml of saturated NH4Cl solution
  3. dry with materialdried over Na2SO4
  4. customevaporated to dryness on a rotavapor

出典と根拠

ORDレコード
ord-91ea94b8d4124a3dbed2cbc620bf0ce1
出典データセット
uspto-grants-2013_12
特許番号
US08617524B2

反応ノート

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