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1-Hydroxybenzotriazole → HCID 68797990、化合物

HRID 1375386
ノート
印刷プレビュー

反応式

HRID 1375386 の反応式
[Cl:1][C:2]1[CH:30]=[C:29]([N:31]2[CH:35]=[CH:34][C:33]([CH3:36])=[N:32]2)[CH:28]=[CH:27][C:3]=1[C:4]([N:6]1[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=2/[C:10](=[CH:17]/[C:18]([NH:20][CH2:21][C:22](O)=[O:23])=[O:19])/[C:9]([F:26])([F:25])[CH2:8][CH2:7]1)=[O:5].C1C=CC2N(O)N=[N:43][C:41]=2C=1.CCN=C=NCCCN(C)C.Cl.CN.C1COCC1.C([O-])(O)=O.[Na+]>C1COCC1>[Cl:1][C:2]1[CH:30]=[C:29]([N:31]2[CH:35]=[CH:34][C:33]([CH3:36])=[N:32]2)[CH:28]=[CH:27][C:3]=1[C:4]([N:6]1[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=2/[C:10](=[CH:17]/[C:18]([NH:20][CH2:21][C:22]([NH:43][CH3:41])=[O:23])=[O:19])/[C:9]([F:26])([F:25])[CH2:8][CH2:7]1)=[O:5]
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 5

HCID 757711-HydroxybenzotriazoleHCID 516892Sodium BicarbonateHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 44520870HCID 44520870、化合物HCID 66615946Methylamine tetrahydrofuran

生成物 1

HCID 68797990HCID 68797990、化合物
収率 19.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 258 mg of the compound of Example 10, 71 mg of HOBt and 101 mg of EDCI.HCl in 5 ml of THF, and 0.5 ml of 2.0 M methylamine-THF solution were added, and the mixture was stirred at room temperature overnight. The reaction solution was mixed with saturated NaHCO3 aq. and extracted with chloroform. The organic layer was dried over anhydrous magnesium sulfate. The crude product obtained by evaporation of the solvent was purified by silica gel column chromatography (chloroform-MeOH (30:1)). The residue obtained by concentration under reduced pressure was crystallized from a 2-propanol-hexane solvent mixture to obtain 51 mg of (2Z)-2-{1-[2-chloro-4-(3-methyl-1H-pyrazol-1-yl)benzoyl]-4,4-difluoro-1,2,3,4-tetrahydro-5H-1-benzazepin-5-ylidene}-N-[2-(methylamino)-2-oxoethyl]acetamide.

後処理

  1. extractionextracted with chloroform
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. customThe crude product obtained by evaporation of the solvent
  4. customwas purified by silica gel column chromatography (chloroform-MeOH (30:1))
  5. customThe residue obtained by concentration under reduced pressure
  6. customwas crystallized from a 2-propanol-hexane solvent mixture

出典と根拠

ORDレコード
ord-6dccc9f7f5be40ab8c00b2c509096445
出典データセット
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07169772B2

反応ノート

読み込み中…

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