1-Hydroxybenzotriazole → HCID 67424004, 화합물

HRID 1393011노트

반응식

HRID 1393011 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

HCID 67424004HCID 67424004, 화합물수율 72.3%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8028Tetrahydrofuran용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-50d8f7b91f2542d2b02ba0e75d4a9d9a
출처 데이터셋
uspto-grants-2008_03
특허 번호
US07345034B2

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