Hydroxyamine hydrochloride → HCID 58420951、化合物

HRID 2178646ノート

反応式

HRID 2178646 の反応式
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]1[S:7][C:8]([CH:11]=O)=[CH:9][N:10]=1.Cl.[NH2:14]O>CN(C)C=O>[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]1[S:7][C:8]([C:11]#[N:14])=[CH:9][N:10]=1

参加物

4

反応物 2

HCID 443297Hydroxyamine hydrochlorideHCID 235606552-(Thiophen-2-yl)-1,3-thiazole-5-carbaldehyde

生成物 1

HCID 58420951HCID 58420951、化合物収率 72.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

6.6 g 2-thiophen-2-yl-thiazole-5-carbaldehyde, 2.8 g hydroxylamine hydrochloride in 45 ml dimethylformamide are heated to 150° C. for 2 hours. The solvent is removed under reduced pressure. The crude product is purified by flash column chromatography in ethylacetate:hexane=1:5. 4.7 g of 2-thiophen-2-yl-thiazole-5-carbonitrile (11) are obtained. 1H (CDCl3): 8.2, 1H, d; 7.6, 1H, d; 7.5, 1H, d; 7.1, 1H, dd. 13C (CDCL3) 166.8 Cq, 152.5 Cq, 135.6 CH, 130.7 CH, 129.0 CH, 128.5 CH, 111.9 Cq 104.4 Cq.

後処理

  1. customThe solvent is removed under reduced pressure
  2. customThe crude product is purified by flash column chromatography in ethylacetate

出典と根拠

ORDレコード
ord-bd375fcecdd443b38aa3ef8f688fa3f6
出典データセット
uspto-grants-2015_06
特許番号
US09067942B2

反応ノート

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