Tris(hydroxymethyl)aminomethane → N-(2,3-dimethylcyclohexyl)benzo[d][1,3]dioxole-5-carboxamide

HRID 339314

반응식

HRID 339314 반응식
[CH3:1][CH:2]1[CH:7]([CH3:8])[CH2:6][CH2:5][CH2:4][CH:3]1[NH2:9].[O:10]1[C:14]2[CH:15]=[CH:16][C:17]([C:19](O)=[O:20])=[CH:18][C:13]=2[O:12][CH2:11]1.N=C=N.OC1C2N=NNC=2C=CC=1.C(O)C(N)(CO)CO>C(#N)C.ClCCl.CN(C=O)C.C(#N)C>[CH3:1][CH:2]1[CH:7]([CH3:8])[CH2:6][CH2:5][CH2:4][CH:3]1[NH:9][C:19]([C:17]1[CH:16]=[CH:15][C:14]2[O:10][CH2:11][O:12][C:13]=2[CH:18]=1)=[O:20]

참가 물질

9

반응물 5

HCID 6503Tris(hydroxymethyl)aminomethaneHCID 71961,3-Benzodioxole-5-carboxylic acidHCID 1235072,3-DimethylcyclohexylamineHCID 160435CarbodiimideHCID 178418300HCID 178418300, 화합물

생성물 1

HCID 17479454N-(2,3-dimethylcyclohexyl)benzo[d][1,3]dioxole-5-carboxamide

시약·촉매·용매 3

HCID 6228Dimethylformamide용매HCID 6342Acetonitrile용매HCID 21877088Acetonitrile methylene chloride용매

실험 절차

2,3-dimethylcyclohexanamine (20 μmol) and benzo[d][1,3]dioxole-5-carboxylic acid (1.1 eq) were each dissolved in acetonitrile/dichloromethane (200 μL, 2:1). PS-Carbodiimide resin (2 eq) was loaded into a 1.2 mL 96 well Greiner plate, followed by the addition of amine and acid solutions. Hydroxybenzotriazole (1.1 eq) was dissolved in DMF (100 mL) and was added into the reaction well. The reaction was shaken overnight at room temperature. Once the reaction was completed, PS-Trisamine resin (1.5 eq) was added into the reaction mixture and the solution was allowed to shake overnight at room temperature. Acetonitrile (200 mL) was added into the reaction well, and the top clear solution was transferred into a new plate. The solution was evaporated to give N-(2,3-dimethylcyclohexyl)benzo[d][1,3]dioxole-5-carboxamide. MS (M+H, 276.20).

후처리

  1. additionwas added into the reaction well
  2. waitto shake overnight at room temperature
  3. customThe solution was evaporated

출처 및 근거

ORD 기록
ord-214d46e93fd848efac87ce532459a3b5
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08895050B2

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