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Triethylamine → HCID 18625984、化合物

HRID 1860091
ノート
印刷プレビュー

反応式

HRID 1860091 の反応式
CS([Cl:5])(=O)=O.C(N(CC)CC)C.[N:13]1[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=1[C:19]1[CH:38]=[CH:37][C:22]([C:23]([NH:25][CH2:26][CH2:27][CH2:28][C:29]2[CH:36]=[CH:35][C:32]([CH2:33]O)=[CH:31][CH:30]=2)=[O:24])=[CH:21][CH:20]=1>ClCCl>[N:13]1[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=1[C:19]1[CH:38]=[CH:37][C:22]([C:23]([NH:25][CH2:26][CH2:27][CH2:28][C:29]2[CH:36]=[CH:35][C:32]([CH2:33][Cl:5])=[CH:31][CH:30]=2)=[O:24])=[CH:21][CH:20]=1
参加物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 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 18625863HCID 18625863、化合物

生成物 1

HCID 18625984HCID 18625984、化合物収率 87.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Methanesulfonyl chloride (294 mg) and triethylamine (0.37 ml) were successively added to a solution of 4-[3-(4-pyridine-2-ylbenzoylamino)propyl]benzylalcohol (0.74 g) in dichloromethane (20 ml). The mixture was allowed to stand at ambient temperature for 16 hours. The reaction mixture was concentrated. The residue was partitioned between ethyl acetate and water. The ethyl acetate layer was separated and washed with saturated aqueous sodium chloride solution and dried over anhydrous magnesium sulfate and concentrated to afford crystals. The crystals were washed with a small amount of diisopropyl ether to afford the desired compound (0.68 g).

後処理

  1. concentrationThe reaction mixture was concentrated
  2. customThe residue was partitioned between ethyl acetate and water
  3. customThe ethyl acetate layer was separated
  4. washwashed with saturated aqueous sodium chloride solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated
  7. customto afford crystals
  8. washThe crystals were washed with a small amount of diisopropyl ether

出典と根拠

ORDレコード
ord-ac7ee40b11a04bc29c729cf9caed018c
出典データセット
uspto-grants-2003_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06528525B1

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート