Tetrahydrofuran → HCID 136060802、化合物

HRID 1851505ノート

反応式

HRID 1851505 の反応式
[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]

参加物

6

反応物 4

HCID 8028TetrahydrofuranHCID 61221Dibutyltin oxideHCID 78378AzidotrimethylsilaneHCID 57901755HCID 57901755、化合物

生成物 1

HCID 136060802HCID 136060802、化合物収率 23%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-d3c9932f76f8462481dc68b8a00aa6a3
出典データセット
uspto-grants-2015_02
特許番号
US08957070B2

反応ノート

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