1-Hydroxybenzotriazole → HCID 67424004、化合物

HRID 1393011ノート

反応式

HRID 1393011 の反応式
[CH3:1][NH:2][CH:3]1[CH2:16][C:15]2[C:6]([CH3:25])([CH:7]3[CH:12]([CH2:13][CH:14]=2)[CH:11]2[CH2:17][CH2:18][CH:19]4[CH:20]([CH3:24])[N:21]([CH3:23])[CH2:22][C:10]24[CH2:9][CH2:8]3)[CH2:5][CH2:4]1.[C:26]([N:33]([CH3:41])[C@@H:34]([C:38]([OH:40])=O)[CH:35]([CH3:37])[CH3:36])([O:28][C:29]([CH3:32])([CH3:31])[CH3:30])=[O:27].Cl.CN(C)CCCN=C=NCC.ON1C2C=CC=CC=2N=N1>C1COCC1.ClCCl>[C:29]([O:28][C:26](=[O:27])[N:33]([CH3:41])[CH:34]([C:38](=[O:40])[N:2]([CH3:1])[CH:3]1[CH2:16][C:15]2[C:6]([CH3:25])([CH:7]3[CH:12]([CH2:13][CH:14]=2)[CH:11]2[CH2:17][CH2:18][CH:19]4[CH:20]([CH3:24])[N:21]([CH3:23])[CH2:22][C:10]24[CH2:9][CH2:8]3)[CH2:5][CH2:4]1)[CH:35]([CH3:36])[CH3:37])([CH3:30])([CH3:31])[CH3:32]

参加物

7

反応物 4

HCID 757711-HydroxybenzotriazoleHCID 551434KurchineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 7018800Boc-N-methyl-D-Valine

生成物 1

HCID 67424004HCID 67424004、化合物収率 72.3%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of compound 7B (240 mg, 0.702 mmol), Boc-N-methyl-D-valine (176 mg, 0.762 mmol), 1-[3-(dimethylamino)propyl]-3-ethylcarbodiimide hydrochloride (208 mg, 1.085 mmol), 1-hydroxybenzotriazole (146 mg, 1.085 mmol), dichloromethane (5 mL) and THF (2.5 mL) was stirred at room temperature overnight. The solvent was evaporated under reduced pressure and the residue was dissolved in minimum amount of dichloromethane and purified on silica gel column, which was eluted with 0.5% ammonium hydroxide and 5% methanol in dichloromethane to give the desired product (282 mg, 72% yield).

後処理

  1. customThe solvent was evaporated under reduced pressure
  2. dissolutionthe residue was dissolved in minimum amount of dichloromethane
  3. custompurified on silica gel column, which
  4. washwas eluted with 0.5% ammonium hydroxide and 5% methanol in dichloromethane

出典と根拠

ORDレコード
ord-50d8f7b91f2542d2b02ba0e75d4a9d9a
出典データセット
uspto-grants-2008_03
特許番号
US07345034B2

反応ノート

読み込み中…