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Dabco → Ethanethioic acid, S-[(diphenylphosphino)methyl] ester

HRID 488893
ノート
印刷プレビュー

反応式

HRID 488893 の反応式
B.[C:2]1([P:8]([CH2:15][S:16][C:17](=[O:19])[CH3:18])[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C1N2CCN(CC2)C1>C1(C)C=CC=CC=1>[C:2]1([P:8]([CH2:15][S:16][C:17](=[O:19])[CH3:18])[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=2)[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=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

4

反応物 2

HCID 9237DabcoHCID 178419194HCID 178419194、化合物

生成物 1

HCID 11266196Ethanethioic acid, S-[(diphenylphosphino)methyl] ester収率 95%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
40 °C

実験手順

Compound 10b (4.00 g, 13.9 mmol) was dissolved in toluene (0.14 L) under Ar(g). DABCO (1.56 g, 13.9 mmol) was added, and the mixture was heated at 40° C. for 4 h. Solvent was removed under reduced pressure, and the residue was dissolved in CH2Cl2 and washed with both 1 N HCl and saturated brine. The organic layer was dried over MgSO4(s), and the solvent was removed under reduced pressure. Compound 11b was isolated in 95% yield, and was used without further purification. Spectral Data. As reported previously.4b

後処理

  1. customSolvent was removed under reduced pressure
  2. dissolutionthe residue was dissolved in CH2Cl2
  3. washwashed with both 1 N HCl and saturated brine
  4. dry with materialThe organic layer was dried over MgSO4(s)
  5. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-75433dfef7c549668436ed6dc735f151
出典データセット
uspto-grants-2005_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06974884B2

反応ノート

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