HCID 22492482, 화합물 → HCID 22492464, 화합물

HRID 351080노트

반응식

HRID 351080 반응식
[OH:1][CH2:2][C:3]#[C:4][C:5]1[CH:6]=[C:7]([S:11]([NH:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)(=[O:13])=[O:12])[CH:8]=[CH:9][CH:10]=1>CC(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C=CC=CC1=2)=O.C(Cl)Cl>[O:1]=[CH:2][C:3]#[C:4][C:5]1[CH:6]=[C:7]([S:11]([NH:14][C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=2)(=[O:13])=[O:12])[CH:8]=[CH:9][CH:10]=1

참가 물질

4

반응물 1

HCID 22492482HCID 22492482, 화합물

생성물 1

HCID 22492464HCID 22492464, 화합물수율 86.7%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 159087Triacetoxyperiodinane용매

실험 절차

3-(3-Hydroxyprop-1-ynyl)-N-phenylbenzenesulfonamide (53a) (0.55 g, 1.9 mmol) was dissolved in a solution of Dess-Martin reagent in methylene chloride (0.157 g/ml) (8.2 ml) and the resultant mixture was stirred at ambient temperature for 30 min. The mixture was partitioned between water (50 ml) and ether (50 ml), and ether solution was washed successively with 5% Na2CO3, water, and dried (Na2SO4). The solvents were removed under reduced pressure to give the title compound (0.47 g, 72%) as an oil. The crude product 54a was used in the further step without an additional purification. 1H NMR (DMSO-d6, HMDSO) δ: 6.96–7.41 (5H, m, C6H5); 7.54–8.07 (4H, m, C6H4); 9.45 (1H, s, CH); 10.41 (1H, s, NH).

후처리

  1. customThe mixture was partitioned between water (50 ml) and ether (50 ml), and ether solution
  2. washwas washed successively with 5% Na2CO3, water
  3. dry with materialdried (Na2SO4)
  4. customThe solvents were removed under reduced pressure

출처 및 근거

ORD 기록
ord-b789970a94b84fe8b0d3c3e7f530fde8
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07183298B2

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