Phentermine → HCID 18977226, 화합물

HRID 2393760노트

반응식

HRID 2393760 반응식
[CH3:1][C:2]([NH2:11])([CH3:10])[CH2:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.C(N([CH2:17][CH3:18])CC)C.[C:19]1(C)[CH:24]=C[C:22]([S:25](Cl)(=[O:27])=[O:26])=[CH:21][CH:20]=1>C(Cl)Cl>[C:17]1([CH3:18])[C:22]([S:25]([NH:11][C:2]([CH3:1])([CH3:10])[CH2:3][C:4]2[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=2)(=[O:27])=[O:26])=[CH:21][CH:20]=[CH:19][CH:24]=1

참가 물질

5

반응물 3

HCID 4771PhentermineHCID 73974-Toluenesulfonyl chlorideHCID 8471Triethylamine

생성물 1

HCID 18977226HCID 18977226, 화합물수율 99.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a nitrogen-blanketed solution of 1,1-dimethyl-2-phenyl-ethylamine (3.56 g, 0.019 mol), methylene chloride (CH2Cl2, 20 mL) and triethylamine (Et3N, 8.01 mL, 0.058 mol) was added para-toluenesulfonyl chloride (TsCl, 4.39 g, 0.023 mol). The mixture was stirred at room temperature for 12 hours while monitoring by gas chromatography. The reaction mixture was partitioned between methylene chloride (100 mL) and water (100 mL) and the organic layer was separated and dried over sodium sulfate. The drying agent was filtered off and the filtrate was concentrated to give 5.73 g of N-toluenesulfonyl-1,1-dimethyl-2-phenyl-ethylamine (yield=99%).

후처리

  1. customThe reaction mixture was partitioned between methylene chloride (100 mL) and water (100 mL)
  2. customthe organic layer was separated
  3. dry with materialdried over sodium sulfate
  4. filtrationThe drying agent was filtered off
  5. concentrationthe filtrate was concentrated

출처 및 근거

ORD 기록
ord-5e094dcbffe74aa6aa0db5ff9727a12f
출처 데이터셋
uspto-grants-1998_09
특허 번호
US05808071

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