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Potassium Carbonate → HCID 131729651、化合物

HRID 1695303
ノート
印刷プレビュー

反応式

HRID 1695303 の反応式
[CH3:1]/[CH:2]=[C:3]1/[CH2:4][CH:5]2[N:16]([CH2:17]/1)[C:14](=[O:15])[C:13]1[C:8](=[CH:9][C:10]([OH:20])=[C:11]([O:18][CH3:19])[CH:12]=1)[N:7]=[CH:6]2.[C:21](=[O:24])([O-])[O-].[K+].[K+].[C:27]([O:31][C:32]([NH:34][CH2:35][CH2:36][CH2:37][O:38][C:39]1[CH:44]=[C:43]([CH2:45][O:46]S(C2C=CC(C)=CC=2)(=O)=O)[N:42]=[C:41]([CH2:57]OS(C2C=CC(C)=CC=2)(=O)=O)[CH:40]=1)=[O:33])([CH3:30])([CH3:29])[CH3:28]>CN(C)C=O.[I-].[K+]>[C:27]([O:31][C:32]([NH:34][CH2:35][CH2:36][CH2:37][O:38][C:39]1[CH:40]=[C:41]([CH2:57][O:20][C:10]2[C:11]([O:18][CH3:19])=[CH:12][C:13]3[C:14](=[O:15])[N:16]4[CH2:17][C:3](=[CH:2][CH3:1])[CH2:4][C@H:5]4[CH:6]=[N:7][C:8]=3[CH:9]=2)[N:42]=[C:43]([CH2:45][O:46][C:10]2[C:11]([O:24][CH3:21])=[CH:12][C:13]3[C:14](=[O:15])[N:16]4[CH2:17][C:3](=[CH:2][CH3:1])[CH2:4][C@H:5]4[CH:6]=[N:7][C:8]=3[CH:9]=2)[CH:44]=1)=[O:33])([CH3:28])([CH3:29])[CH3:30]
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

6

反応物 3

HCID 11430Potassium CarbonateHCID 5856240PRETOMAYMYCINHCID 71496931HCID 71496931、化合物

生成物 1

HCID 131729651HCID 131729651、化合物収率 18.4%

試薬・触媒・溶媒 2

HCID 4875Potassium Iodide溶媒HCID 6228
Dimethylformamide
溶媒
2 回

反応条件

温度
30 °C

実験手順

To a stirred solution of pre-tomaymycin (30 mg) in dimethylformamide (0.5 mL), were added potassium carbonate (45.7 mg), a solution of 4-(3-tert-butoxycarbonylamino-propoxy)-2,6-bis-(tosyloxymethyl)-pyridine (41 mg) in dimethylformamide (0.5 mL) and potassium iodide (18.3 mg). The reaction was stirred for 20 h at 30° C. Solids were filtered off and washed with dimethylformamide (0.2 mL). Water (0.5 mL) was added to the combined dimethylformamide solution and formic acid was added until complete dissolution of the precipitate. The resulting solution was injected for HPLC purification according to method B1. The appropriate fractions were combined and concentrated by centrifugal evaporation over a Jouan Model RC10.10. apparatus to afford 8,8′-[4-(3-tert-butoxycarbonylaminopropyloxy)-2,6-pyridine-diylbis(methylenoxy)]-bis[(S)-2-eth-(E)-ylidene-7-methoxy-1,2,3,11a-tetrahydro-5H-pyrrolo[2,1-c][1,4]benzodiazepin-5-one] (8.3 mg).

後処理

  1. filtrationSolids were filtered off
  2. washwashed with dimethylformamide (0.2 mL)
  3. additionWater (0.5 mL) was added to the combined dimethylformamide solution and formic acid
  4. additionwas added until complete dissolution of the precipitate
  5. customThe resulting solution was injected for HPLC purification
  6. concentrationconcentrated by centrifugal evaporation over a Jouan Model RC10.10

出典と根拠

ORDレコード
ord-7b69c926b35c453682abf1e131e0ad0c
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08163736B2

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