Triethylamine → HCID 68881182, 화합물

HRID 915904노트

반응식

HRID 915904 반응식
[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

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 68880923HCID 68880923, 화합물

생성물 1

HCID 68881182HCID 68881182, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7786f7818b24484b96c2d24998eac6d3
출처 데이터셋
uspto-grants-2007_09
특허 번호
US07268151B2

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