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Thiourea → s-(2-Cyanomethylphenyl)methylisothiourea hydrochloride

HRID 2196464
ノート
印刷プレビュー

反応式

HRID 2196464 の反応式
[Cl:1][CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[CH2:9][C:10]#[N:11].[NH2:12][C:13]([NH2:15])=[S:14]>CO>[ClH:1].[C:10]([CH2:9][C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=1[CH2:2][S:14][C:13](=[NH:12])[NH2:15])#[N:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 2723790ThioureaHCID 112981592-(Cyanomethyl)benzyl chloride

生成物 1

HCID 66818824s-(2-Cyanomethylphenyl)methylisothiourea hydrochloride収率 79%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

The 2-chlormethylphenylacetonitrile (200 mg, 1.21 mmol) and thiourea (101 mg, 1.33 mmol) were mixed in 1 ml of methanol. The mixture was heated to reflux for 3 to 4 hours. The reaction mixture was evaporated. After that, 1 ml of methanol and 4 ml of acetone were added and the mixture was stirred for one hour. The crystalline material was filtered and the product was dried under high vacuum overnight to yield 231 mg (0.95 mmol, yield 79%) of product as off white crystals, with purity greater than 95%. 1H NMR (300 MHz, d6-DMSO) δ 4.14 (s, 2H), 4.56 (s, 2H), 7.37 (m, 2H), 7.45 (m, 2H), 9.23 (s, 4H). (M+H) 205.97

後処理

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 3 to 4 hours
  3. customThe reaction mixture was evaporated
  4. additionAfter that, 1 ml of methanol and 4 ml of acetone were added
  5. filtrationThe crystalline material was filtered
  6. customthe product was dried under high vacuum overnight

出典と根拠

ORDレコード
ord-45742ca247d04703888157a61cefe840
出典データセット
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08338454B2

反応ノート

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