Tert-Butylamine → HCID 13178322、化合物

HRID 1074371

反応式

HRID 1074371 の反応式
[C:1]([NH2:5])([CH3:4])([CH3:3])[CH3:2].[S:6]1[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[C:8]([S:15](Cl)(=[O:17])=[O:16])=[CH:7]1>O1CCCC1>[C:1]([NH:5][S:15]([C:8]1[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[S:6][CH:7]=1)(=[O:16])=[O:17])([CH3:4])([CH3:3])[CH3:2]

参加物

4

反応物 2

HCID 6385Tert-ButylamineHCID 27763401-Benzothiophene-3-sulfonyl chloride

生成物 1

HCID 13178322HCID 13178322、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To 25 g of tert-butyl amine in 100 ml of dry tetrahydrofuran was added dropwise with cooling 34 g of benzothiophene-3-sulfonyl chloride. The reaction mixture was allowed to come to room temperature and then poured into 200 g of ice. The phases were separated and the organic portion was washed with water, dried over magnesium sulfate and evaporated in vacuo. The residue thus obtained melted at 146°-148° after recrystallization from alcohol. It showed an absorption peak by NMR at 1.34 δ (singlet), for tert-butyl and 7.4-8.4 δ (multiplet) for benzothiophene consistent for the desired product.

後処理

  1. customto come to room temperature
  2. customThe phases were separated
  3. washthe organic portion was washed with water
  4. dry with materialdried over magnesium sulfate
  5. customevaporated in vacuo
  6. customThe residue thus obtained melted at 146°-148° after recrystallization from alcohol

出典と根拠

ORDレコード
ord-c5dc0a21952943dbae1a78ce65def847
出典データセット
uspto-grants-1983_07
特許番号
US04391627

関連ノート

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