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Benzenemethanethiol, alpha,alpha-diphenyl- → HCID 68599758、化合物

HRID 2246074
ノート
印刷プレビュー

反応式

HRID 2246074 の反応式
[C:1]([C:3]1[S:7][CH:6]=[N:5][C:4]=1[CH2:8][OH:9])#[CH:2].[C:10]1([C:16]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[SH:17])[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.CC(C)([O-])C.[K+]>C1COCC1.[Cl-].[Na+].O>[OH:9][CH2:8][C:4]1[N:5]=[CH:6][S:7][C:3]=1/[CH:1]=[CH:2]\[S:17][C:16]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)([C:24]1[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=1)[C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 77281Benzenemethanethiol, alpha,alpha-diphenyl-HCID 23665647Potassium tert-butoxideHCID 45121755HCID 45121755、化合物

生成物 1

HCID 68599758HCID 68599758、化合物

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 57417360Sodium chloride; water溶媒

実験手順

A solution of 2.73 g of 5-ethynyl-4-hydroxymethylthiazole in 65 ml of THF was cooled in ice under an argon atmosphere, and 6.5 g of triphenylmethane thiol and 440 mg of potassium-t-butoxide were added to the cooled solution. The mixture was stirred at room temperature for 2 hr. Brine was added to the reaction solution, and the mixture was extracted twice with ethyl acetate. The organic layers were combined, were washed with brine, were then dried over anhydrous magnesium sulfate, were filtered, and were concentrated under the reduced pressure. Ethyl acetate (10 ml) and 10 ml of hexane were added to the residue, and the resultant precipitate was collected by filtration to give 7.26 of the title compound.

後処理

  1. extractionthe mixture was extracted twice with ethyl acetate
  2. washwere washed with brine
  3. dry with materialwere then dried over anhydrous magnesium sulfate
  4. filtrationwere filtered
  5. concentrationwere concentrated under the reduced pressure
  6. additionEthyl acetate (10 ml) and 10 ml of hexane were added to the residue
  7. filtrationthe resultant precipitate was collected by filtration

出典と根拠

ORDレコード
ord-b0068b566c8b4e40aa49123868046e11
出典データセット
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07687490B2

反応ノート

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