Phentermine → HCID 18977226、化合物

HRID 2393760ノート

反応式

HRID 2393760 の反応式
[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

参加物

5

反応物 3

HCID 4771PhentermineHCID 73974-Toluenesulfonyl chlorideHCID 8471Triethylamine

生成物 1

HCID 18977226HCID 18977226、化合物収率 99.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-5e094dcbffe74aa6aa0db5ff9727a12f
出典データセット
uspto-grants-1998_09
特許番号
US05808071

反応ノート

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