Hydroxyamine hydrochloride → HCID 58420951, 화합물

HRID 2178646노트

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HRID 2178646 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 58420951HCID 58420951, 화합물수율 72.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-bd375fcecdd443b38aa3ef8f688fa3f6
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09067942B2

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