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Diethyl [chloro(4-chlorophenyl)methyl]phosphonate → 2-[5-(4-Chlorophenylethynyl)thien-2-ylethynyl]benzothiophene

HRID 1460994
ノート
印刷プレビュー

反応式

HRID 1460994 の反応式
[CH:1]([C:3]1[S:7][C:6]([C:8]#[C:9][C:10]2[S:11][C:12]3[CH:18]=[CH:17][CH:16]=[CH:15][C:13]=3[CH:14]=2)=[CH:5][CH:4]=1)=O.[Cl:19][C:20]1[CH:25]=[CH:24][C:23]([CH:26](P(=O)(OCC)OCC)Cl)=[CH:22][CH:21]=1.CC(C)([O-])C.[K+]>CN(C)C=O>[Cl:19][C:20]1[CH:25]=[CH:24][C:23]([C:26]#[C:1][C:3]2[S:7][C:6]([C:8]#[C:9][C:10]3[S:11][C:12]4[CH:18]=[CH:17][CH:16]=[CH:15][C:13]=4[CH:14]=3)=[CH:5][CH:4]=2)=[CH:22][CH:21]=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

5

反応物 3

HCID 12881548Diethyl [chloro(4-chlorophenyl)methyl]phosphonateHCID 199814132-(5-Formylthien-2-ylethynyl)benzothiopheneHCID 23665647Potassium tert-butoxide

生成物 1

HCID 199814142-[5-(4-Chlorophenylethynyl)thien-2-ylethynyl]benzothiophene収率 19.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
0 °C

実験手順

A stirred solution of 0.75 gram (0.0028 mole) of 2-(5-formylthien-2-ylethynyl)benzothiophene and 0.83 gram (0.0028 mole) of diethyl (4-chlorophenyl)chloromethylphosphonate in 10 ml of dimethylformamide was cooled to 0° C., and 0.94 gram (0.0084 mole) of potassium tertbutoxide was added. Upon completion of addition, the reaction mixture was stirred at 0° C. for 30 minutes and then was allowed to warm to ambient temperature where it was stirred for 18 hours. After this time the reaction mixture was subjected to column chromatography on silica gel. Elution was accomplished using hexane. The appropriate fractions were combined and concentrated under reduced pressure, yielding 0.20 gram of 2-[5-(4-chlorophenylethynyl)thien-2-ylethynyl]benzothiophene; m.p. 189°-191° C. The nmr spectrum was consistent with the proposed structure.

後処理

  1. additionUpon completion of addition
  2. temperatureto warm to ambient temperature where it
  3. stirringwas stirred for 18 hours
  4. washElution
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-e6ff885b78e642bc83fdfeade4a57314
出典データセット
uspto-grants-1991_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05073564

反応ノート

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