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Acetyl chloride → 2-[4-(6-Fluoro-1,2-benzisoxazol-yl)-piperidinyl]ethyl acetamide fumarate

HRID 233208
ノート
印刷プレビュー

反応式

HRID 233208 の反応式
[F:1][C:2]1[CH:19]=[CH:18][C:5]2[C:6]([CH:9]3[CH2:14][CH2:13][N:12]([CH2:15][CH2:16]N)[CH2:11][CH2:10]3)=[N:7][O:8][C:4]=2[CH:3]=1.[CH2:20]([N:22](CC)CC)[CH3:21].C(Cl)(=[O:29])C.[C:31]([OH:38])(=[O:37])/[CH:32]=[CH:33]/[C:34]([OH:36])=[O:35]>C(Cl)Cl.C(O)C>[C:31]([OH:38])(=[O:37])/[CH:32]=[CH:33]/[C:34]([OH:36])=[O:35].[F:1][C:2]1[CH:19]=[CH:18][C:5]2[C:6]([CH:9]3[CH2:10][CH2:11][N:12]([CH2:15][CH2:16][CH2:21][C:20]([NH2:22])=[O:29])[CH2:13][CH2:14]3)=[N:7][O:8][C:4]=2[CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 444972Fumaric AcidHCID 146998572-(4-(6-Fluorobenzo[d]isoxazol-3-yl)piperidin-1-yl)ethan-1-amine

生成物 1

HCID 867482572-[4-(6-Fluoro-1,2-benzisoxazol-yl)-piperidinyl]ethyl acetamide fumarate

試薬・触媒・溶媒 2

HCID 702
Ethanol
溶媒
HCID 6344Dichloromethane溶媒2 回

実験手順

A mixture of 2-[4-(6-fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]ethylamine (2.56 g, 9.7 mmol) and triethylamine (1.45 g, 14.5 mmol) in DCM (50 ml) was treated with dropwise addition of acetyl chloride (1.0 g, 12.7 mmol) at room temperature. The mixture was stirred for 4 hours at room temperature. The reaction mixture was diluted with DCM and washed with brine. The organic solution was dried over MgSO4 and concentrated to a crude oil. The crude oil was purified by flash chromatography over a silica gel column (SiO2, 20 g; eluted with (0-2%) CH3OH in DCM). The pure product thus obtained weighed 1.36 g (46%). It was converted to a fumarate salt by treatment with fumaric acid (517 mg) in ethanol. Recrystallization from ethanol gave white crystals; weight: 1.53 g, m.p.=132°-133° C.

後処理

  1. washwashed with brine
  2. dry with materialThe organic solution was dried over MgSO4
  3. concentrationconcentrated to a crude oil
  4. customThe crude oil was purified by flash chromatography over a silica gel column (SiO2, 20 g; eluted with (0-2%) CH3OH in DCM)
  5. customThe pure product thus obtained
  6. customRecrystallization from ethanol
  7. customgave white crystals

出典と根拠

ORDレコード
ord-b08e0f21a0f8414f815352566e6cec9b
出典データセット
uspto-grants-1997_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05591745

反応ノート

読み込み中…

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