Triethylamine → HCID 53655042、化合物

HRID 1003823ノート

反応式

HRID 1003823 の反応式
[OH:1][CH2:2][CH2:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([C:11](=[O:20])[CH2:12][CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[CH:7][CH:6]=1.C(N(CC)CC)C.[S:28](Cl)([CH3:31])(=[O:30])=[O:29]>C(Cl)Cl>[C:14]1([CH2:13][CH2:12][C:11]([C:8]2[CH:9]=[CH:10][C:5]([O:4][CH2:3][CH2:2][O:1][S:28]([CH3:31])(=[O:30])=[O:29])=[CH:6][CH:7]=2)=[O:20])[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 187986891-[4-(2-Hydroxy-ethoxy)-phenyl]-3-phenyl-propan-1-one

生成物 1

HCID 53655042HCID 53655042、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of 1-[4-(2-hydroxy-ethoxy)-phenyl]-3-phenyl-propan-1-one (prepared in Example N; 6.0 g, 22.2 mmol) and triethylamine (NEt3) (4.60 mL, 33.3 mmol) in CH2Cl2 (50 mL) was cooled to 0° C. under a nitrogen atmosphere and treated with mesyl chloride (2.1 mL, 26.6 mmol). The mixture allowed to stir for 45 minutes, and then diluted with additional CH2Cl2 and washed with H2O. The organic layer was dried (MgSO4) and the solvent removed in vacuo to provide the title compound which was used without further purification. 1H NMR (DMSO-d6) δ 2.90 (t, 2 H), 3.20 (s, 3 H), 3.29 (t, 2 H), 4.32-4.34 (m, 2 H), 4.52-4.55 (m, 2 H), 7.05 (d, 2 H), 7.22-7.32 (m, 5 H), 7.95 (d, 2 H).

後処理

  1. washwashed with H2O
  2. dry with materialThe organic layer was dried (MgSO4)
  3. customthe solvent removed in vacuo

出典と根拠

ORDレコード
ord-e8c97de80d8a4a2c874cef9d2eb4b4f9
出典データセット
uspto-grants-2000_04
特許番号
US06046355

反応ノート

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