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Potassium Carbonate → HCID 68677180、化合物

HRID 1158512
ノート
印刷プレビュー

反応式

HRID 1158512 の反応式
[CH3:1][O:2][C:3](=[O:41])[NH:4][C@H:5]([C:10]([NH:12][NH:13][CH2:14][CH2:15][C@:16]([CH2:34][C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1)([OH:33])[C:17]([N:19]1[C@H:23]2[C:24]3[CH:25]=[CH:26][CH:27]=[CH:28][C:29]=3[CH2:30][C@H:22]2[O:21]C1(C)C)=[O:18])=[O:11])[C:6]([CH3:9])([CH3:8])[CH3:7].C([O-])([O-])=O.[K+].[K+].[Br:48][C:49]1[CH:56]=[CH:55][C:52]([CH2:53]Br)=[CH:51][CH:50]=1>CC(=O)CC>[CH3:1][O:2][C:3](=[O:41])[NH:4][C@@H:5]([C:10]([NH:12][N:13]([CH2:53][C:52]1[CH:55]=[CH:56][C:49]([Br:48])=[CH:50][CH:51]=1)[CH2:14][CH2:15][C@@:16]([OH:33])([C:17](=[O:18])[NH:19][C@H:23]1[C:24]2[C:29](=[CH:28][CH:27]=[CH:26][CH:25]=2)[CH2:30][C@H:22]1[OH:21])[CH2:34][C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1)=[O:11])[C:6]([CH3:7])([CH3:9])[CH3:8]
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

5

反応物 3

HCID 11430Potassium CarbonateHCID 685274-Bromobenzyl bromideHCID 68676597HCID 68676597、化合物

生成物 1

HCID 68677180HCID 68677180、化合物

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

反応条件

温度
80 °C

実験手順

Compound 21i (0.105 g) was dissolved in 2-butanone (10 mL) and added K2CO3 (0.045 g, 0.32 mmol), and 4-bromobenzyl bromide (0.054 g, 0.21 mmol) and stirred at 80° C. for 3 h. Solvent was evaporated and the residue was dissolved in dichloromethane (15 mL), washed with water, brine and cooled to 0° C. TFA (1.0 mL) was added slowly and stirred for 30 min then evaporated. Residue dissolved in dichloromethane (10 mL) and washed with NaHCO3 solution, water, brine and dried. Residue was purified by analytical preparative LCMS to yield 0.023 g (15% overall yield) of the title compound.

後処理

  1. customSolvent was evaporated
  2. dissolutionthe residue was dissolved in dichloromethane (15 mL)
  3. washwashed with water, brine
  4. temperaturecooled to 0° C
  5. additionTFA (1.0 mL) was added slowly
  6. stirringstirred for 30 min
  7. customthen evaporated
  8. dissolutionResidue dissolved in dichloromethane (10 mL)
  9. washwashed with NaHCO3 solution, water, brine
  10. customdried
  11. customResidue was purified by analytical preparative LCMS
  12. customto yield

出典と根拠

ORDレコード
ord-a0e74bf6989d48b1af6572493d9a6286
出典データセット
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07807677B2

反応ノート

読み込み中…

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