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Dimethyl Sulfoxide → HCID 53890318、化合物

HRID 263543
ノート
印刷プレビュー

反応式

HRID 263543 の反応式
CS(C)=O.C(Cl)(=O)C(Cl)=O.[C:11]1([C:17]2[C:25]([CH:26]=[CH:27][C:28]([N:30]3[CH2:35][CH2:34][CH2:33][CH2:32][C@@H:31]3[CH2:36][CH2:37][OH:38])=[O:29])=[C:20]3[CH:21]=[CH:22][CH:23]=[CH:24][N:19]3[N:18]=2)[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.[Cl-].[NH4+]>C(Cl)Cl.C(N(CC)CC)C>[C:11]1([C:17]2[C:25]([CH:26]=[CH:27][C:28]([N:30]3[CH2:35][CH2:34][CH2:33][CH2:32][C@@H:31]3[CH2:36][CH:37]=[O:38])=[O:29])=[C:20]3[CH:21]=[CH:22][CH:23]=[CH:24][N:19]3[N:18]=2)[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 679Dimethyl SulfoxideHCID 25517Ammonium ChlorideHCID 65578Oxalyl chlorideHCID 129453HCID 129453、化合物

生成物 1

HCID 53890318HCID 53890318、化合物収率 38.4%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒3 回
HCID 8471
Triethylamine
溶媒

反応条件

温度
-45 °C

実験手順

A solution of dimethyl sulfoxide (202 mg) in methylene chloride (1.0 ml) was added dropwise to a solution of oxalyl dichloride (247 mg) in methylene chloride (10 ml) over 5 minutes at -78° C. After 10 minutes, a solution of (2R)-1-[3-(2-phenylpyrazolo[1,5-a]pyridin-3-yl)acryloyl]-2-(2-hydroxyethyl)piperidine (trans isomer) (364 mg) in methylene chloride (3.4 mg) was added dropwise over 10 minutes at -78° C. The solution was stirred at -78° C. for 20 minutes and at -45° C. for 1 hour. Triethylamine (986 μl) was added to the solution and the mixture was stirred at -20°~0° C. for 20 minutes. Saturated ammonium chloride solution (20 ml) was added to the reaction mixture was the mixture was extracted with methylene chloride (10 ml×2). The combined extracts were washed with brine (10 ml), dried over magnesium sulfate and evaporated in vacuo. The crude material was purified by column chromatography on silica gel (10 g) with a mixture of methylene chloride and ethyl acetate (10:1) as an eluent to give (2R)-1-[3-(2-phenylpyrazolo[1,5-a]pyridin-3-yl)acryloyl]-2-(formylmethyl)piperidine (trans isomer) (139.0 mg) as an oil.

後処理

  1. stirringthe mixture was stirred at -20°~0° C. for 20 minutes
  2. extractionwas extracted with methylene chloride (10 ml×2)
  3. washThe combined extracts were washed with brine (10 ml)
  4. dry with materialdried over magnesium sulfate
  5. customevaporated in vacuo
  6. customThe crude material was purified by column chromatography on silica gel (10 g) with a mixture of methylene chloride and ethyl acetate (10:1) as an eluent

出典と根拠

ORDレコード
ord-0243842debe24a93afd3c83bc3407ac2
出典データセット
uspto-grants-1997_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05643938

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート