Tetrahydrofuran → HCID 136060802, 화합물

HRID 1851505노트

반응식

HRID 1851505 반응식
[C:1]([C:3]1[NH:4][C:5]2[C:10]([CH:11]=1)=[CH:9][CH:8]=[CH:7][C:6]=2[NH:12][S:13]([C:16]1[S:17][CH:18]=[CH:19][CH:20]=1)(=[O:15])=[O:14])#[N:2].C[Si]([N:25]=[N+:26]=[N-:27])(C)C.C([Sn](=O)CCCC)CCC.O1CCCC1>C(OCC)(=O)C>[N:2]1[NH:25][N:26]=[N:27][C:1]=1[C:3]1[NH:4][C:5]2[C:10]([CH:11]=1)=[CH:9][CH:8]=[CH:7][C:6]=2[NH:12][S:13]([C:16]1[S:17][CH:18]=[CH:19][CH:20]=1)(=[O:14])=[O:15]

참가 물질

6

반응물 4

HCID 8028TetrahydrofuranHCID 61221Dibutyltin oxideHCID 78378AzidotrimethylsilaneHCID 57901755HCID 57901755, 화합물

생성물 1

HCID 136060802HCID 136060802, 화합물수율 23%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

A mixture of N-(2-cyano-1H-indol-7-yl)thiophene-2-sulfonamide (0.40 g), trimethylsilylazide (0.35 mL), dibutyltin oxide (33 mg) and tetrahydrofuran (15 mL) was heated under reflux overnight. To the reaction mixture was added ethyl acetate, the mixture was ice-cooled, and the resulting crystals were filtrated, washed with cold ethyl acetate, and dried to give the title compound (0.09 g, yield 23%) as pale-yellow crystals. The crystals were recrystallized from ethyl acetate-hexane. melting point 274-275° C. (decomposition).

후처리

  1. temperaturewas heated
  2. temperatureunder reflux overnight
  3. temperaturecooled
  4. filtrationthe resulting crystals were filtrated
  5. washwashed with cold ethyl acetate
  6. customdried

출처 및 근거

ORD 기록
ord-d3c9932f76f8462481dc68b8a00aa6a3
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08957070B2

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