Triethylamine → HCID 68881182、化合物

HRID 915904ノート

反応式

HRID 915904 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:15](O)[CH2:16][N+:17]([O-:19])=[O:18])[CH:6]=[CH:7][C:8]=1[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][N:10]=1.C(N(CC)CC)C.CS(Cl)(=O)=O>ClCCl>[CH3:1][O:2][C:3]1[CH:4]=[C:5](/[CH:15]=[CH:16]\[N+:17]([O-:19])=[O:18])[CH:6]=[CH:7][C:8]=1[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][N:10]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 68880923HCID 68880923、化合物

生成物 1

HCID 68881182HCID 68881182、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 1-(3-methoxy4-pyridin-2-ylphenyl)-2-nitroethanol (290 mg, 1.06 mmol) in anhydrous dichloromethane (5 mL) was treated with triethylamine (0.24 mL, 1.69 mmol), followed by methanesulfonyl chloride (0.10 mL, 1.27 mmol), 1 hr later, the mixture was partitioned between sat. NaHCO3 (10 mL) and dichloromethane (20 mL). The phases were separated and the aqueous layer was extracted with dichloromethane (3×10 mL). The combined organic layers were dried (MgSO4), filtered and concentrated to afford a yellow solid.

後処理

  1. customthe mixture was partitioned between sat. NaHCO3 (10 mL) and dichloromethane (20 mL)
  2. customThe phases were separated
  3. extractionthe aqueous layer was extracted with dichloromethane (3×10 mL)
  4. dry with materialThe combined organic layers were dried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customto afford a yellow solid

出典と根拠

ORDレコード
ord-7786f7818b24484b96c2d24998eac6d3
出典データセット
uspto-grants-2007_09
特許番号
US07268151B2

反応ノート

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