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Potassium Iodide → HCID 21471809、化合物

HRID 2294840
ノート
印刷プレビュー

反応式

HRID 2294840 の反応式
Cl[CH2:2][CH2:3][C:4]1[S:14][C:7]2[C:8](=[O:13])[NH:9][CH2:10][CH2:11][CH2:12][C:6]=2[CH:5]=1.Cl.[F:16][C:17]1[CH:31]=[CH:30][C:20]2[C:21]([CH:24]3[CH2:29][CH2:28][NH:27][CH2:26][CH2:25]3)=[N:22][O:23][C:19]=2[CH:18]=1.C(=O)([O-])[O-].[K+].[K+].[I-].[K+]>CN(C)C=O.C1(C)C=CC=CC=1>[F:16][C:17]1[CH:31]=[CH:30][C:20]2[C:21]([CH:24]3[CH2:25][CH2:26][N:27]([CH2:2][CH2:3][C:4]4[S:14][C:7]5[C:8](=[O:13])[NH:9][CH2:10][CH2:11][CH2:12][C:6]=5[CH:5]=4)[CH2:28][CH2:29]3)=[N:22][O:23][C:19]=2[CH:18]=1
参加物反応条件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 4875Potassium IodideHCID 11430Potassium CarbonateHCID 11334359R-56109 hydrochlorideHCID 21471776HCID 21471776、化合物

生成物 1

HCID 21471809HCID 21471809、化合物収率 45.1%

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒
HCID 6228
Dimethylformamide
溶媒

反応条件

温度
90 °C

実験手順

A mixture of 800 mg of 2-chloroethyl-4,5,6,7-tetrahydro-8H-thieno[2,3-c]azepin-8-one, 920 mg of 4-(6-fluoro-1,2-benzisoxazol-3-yl)piperidine hydrochloride, 1.45 g of potassium carbonate and 580 mg of potassium iodide in 10 ml of dimethylformamide and 10 ml of toluene was stirred at 90° C. for 22 hours and concentrated in vacuo. To the residue were added ethyl acetate and water, and separated. The ethyl acetate layer was washed with water, dried over magnesium sulfate and concentrated in vacuo. The residue was purified by column chromatography on a silica gel and recrystallized from ethyl acetate to give 0.65 g of 2-(2-(4-(6-fluoro-1,2-benzisoxazol-3-yl)piperidin-1-yl)ethyl)-4,5,6,7-tetrahydro-8H-thieno[2,3-c]azepin-8-one, m.p. 192°-194° C.

後処理

  1. concentrationconcentrated in vacuo
  2. additionTo the residue were added ethyl acetate and water
  3. customseparated
  4. washThe ethyl acetate layer was washed with water
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified by column chromatography on a silica gel
  8. customrecrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-9d990a0568674070a183f3d29309839b
出典データセット
uspto-grants-1997_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05691330

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート