Acetic Anhydride → 1-(2,3-Dihydro-1,4-benzothiazepin-4(5H)-yl)ethanone

HRID 1910437ノート

反応式

HRID 1910437 の反応式
[S:1]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[CH2:5][NH:4][CH2:3][CH2:2]1.C(N(CC)CC)C.[C:19](OC(=O)C)(=[O:21])[CH3:20]>ClCCl>[S:1]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[CH2:5][N:4]([C:19](=[O:21])[CH3:20])[CH2:3][CH2:2]1

参加物

5

反応物 3

HCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 122691062,3,4,5-Tetrahydrobenzo[f][1,4]thiazepine

生成物 1

HCID 146707161-(2,3-Dihydro-1,4-benzothiazepin-4(5H)-yl)ethanone収率 100%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 2,3,4,5-tetrahydro-1,4-benzothiazepine (5 g, 30.3 mmol) in dry dichloromethane (100 mL) was added triethylamine (5.06 mL, 36.3 mmol) at room temperature, followed by the addition of acetic anhydride (3.43 mL, 36.3 mmol) dropwise at 0° C. under nitrogen. The resulting solution was stirred for 1 hour whilst allowing the temperature to rise slowly to room temperature. The mixture was washed with brine (50 mL×2), dried over sodium sulfate, filtered and concentrated in vacuo to afford 6.28 g of product as yellow oil, which was used for next step without further purification.

後処理

  1. customto rise slowly to room temperature
  2. washThe mixture was washed with brine (50 mL×2)
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-385c5c827fcd4431925ff99cac654ca1
出典データセット
uspto-grants-2013_12
特許番号
US08604019B2

反応ノート

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