Triethylamine → HCID 21888309、化合物

HRID 1058924ノート

反応式

HRID 1058924 の反応式
C(N(CC)CC)C.[N+:8]([CH2:11][C:12]1([CH2:18][CH2:19][NH2:20])[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]1)([O-:10])=[O:9].[CH3:21][S:22](Cl)(=[O:24])=[O:23]>O1CCCC1>[N+:8]([CH2:11][C:12]1([CH2:18][CH2:19][NH:20][S:22]([CH3:21])(=[O:24])=[O:23])[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]1)([O-:10])=[O:9]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 12970145HCID 12970145、化合物2 回

生成物 1

HCID 21888309HCID 21888309、化合物収率 47.6%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Triethylamine (0.64 g, 6.3 mmol) was added dropwise to a mixture of the amine hydrochloride salt (compound 4, 0.70 g, 3.1 mmol) and methane sulfonyl chloride (0.36 g, 6.3 mmol) in tetrahydrofuran (35 nL). After stirring at room temperature for 2 hours, the mixture was filtered, diluted with ethyl acetate, and washed with dilute hydrochloric acid, saturated sodium bicarbonate solution, and water, dried over magnesium sulphate, filtered, and evaporated to dryness. The residue was crystallized from ethyl acetate/heptane to give colorless crystals (0.39 g, 47%); mp 86-88° C.

後処理

  1. filtrationthe mixture was filtered
  2. additiondiluted with ethyl acetate
  3. washwashed with dilute hydrochloric acid, saturated sodium bicarbonate solution, and water
  4. dry with materialdried over magnesium sulphate
  5. filtrationfiltered
  6. customevaporated to dryness
  7. customThe residue was crystallized from ethyl acetate/heptane

出典と根拠

ORDレコード
ord-7a194c0888ce4a7bb464ea11c8072414
出典データセット
uspto-grants-2003_02
特許番号
US06518289B1

反応ノート

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