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Potassium Carbonate → HCID 22592129、化合物

HRID 746648
ノート
印刷プレビュー

反応式

HRID 746648 の反応式
Br[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][C:10]([NH:12][C:13]1[C:14]([S:22][CH3:23])=[N:15][C:16]([CH3:21])=[CH:17][C:18]=1[S:19][CH3:20])=[O:11].[CH3:24][O:25][C:26]([C:28]1[C:36]2[O:35][C:34]([SH:37])=[N:33][C:32]=2[CH:31]=[CH:30][CH:29]=1)=[O:27].C1OCCOCCOCCOCCOCCOC1.C(=O)([O-])[O-].[K+].[K+]>O.CN(C=O)C>[CH3:24][O:25][C:26]([C:28]1[C:36]2[O:35][C:34]([S:37][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][C:10]([NH:12][C:13]3[C:14]([S:22][CH3:23])=[N:15][C:16]([CH3:21])=[CH:17][C:18]=3[S:19][CH3:20])=[O:11])=[N:33][C:32]=2[CH:31]=[CH:30][CH:29]=1)=[O:27]
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 11430Potassium CarbonateHCID 2855718-Crown-6HCID 22592164HCID 22592164、化合物HCID 178497587HCID 178497587、化合物

生成物 1

HCID 22592129HCID 22592129、化合物収率 72%

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 6228
Dimethylformamide
溶媒

反応条件

温度
80 °C

実験手順

To a DMF (4 ml) solution of 9-bromo-N-[2,4-bis(methylthio)-6-methyl-3-pyridyl]nonanamide (90 mg, 0.22 mmol) and 7-methoxycarbonyl-2-mercaptobenzoxazole (45 mg, 0.22 mmol) were added 18-crown-6 (6 mg, 0.02 mmol) and potassium carbonate (36 mg, 0.26 mmol), and the mixture was stirred at 80° C. for 4 hours. The reaction mixture was diluted with water, and then extracted with ethyl acetate. The organic layer was washed with water and then with a saturated aqueous solution of sodium chloride, and dried over magnesium sulfate. Subsequently, the solvent was distilled off, and the resulting crude product was recrystallized from a mixture of ethyl acetate and hexane to obtain 84 mg (yield 72%) of the desired compound as a colorless powdery crystal.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with water
  3. dry with materialwith a saturated aqueous solution of sodium chloride, and dried over magnesium sulfate
  4. distillationSubsequently, the solvent was distilled off
  5. customthe resulting crude product was recrystallized from a mixture of ethyl acetate and hexane

出典と根拠

ORDレコード
ord-88de6a9a607245318b7bd60fd69cf446
出典データセット
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07393866B2

反応ノート

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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