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HCID 22450431、化合物 → N-methyl-1-(pyridin-2-yl)methanamine

HRID 1954984
ノート
印刷プレビュー

反応式

HRID 1954984 の反応式
CSC(=NC)[N:4]([CH2:6][C:7]1[CH:12]=[CH:11][C:10](Cl)=[CH:9]C=1)[CH3:5].C[NH:17]C(N(C)CC1C=CN=CC=1)=S>[N+](C)([O-])=O>[CH3:5][NH:4][CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][N:17]=1
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 22450431HCID 22450431、化合物HCID 22450450HCID 22450450、化合物

生成物 1

HCID 88757N-methyl-1-(pyridin-2-yl)methanamine

試薬・触媒・溶媒 1

HCID 6375Nitromethane溶媒

実験手順

To 4.98 g (0.0205 mole) of S-methyl-N-(4-chlorobenzyl)-N-methyl-N'-methylisothiourea prepared in (1) was added 25 ml of nitromethane and the mixture was refluxed for 6.5 hours. The nitromethane was distilled off and the residue was subjected to silica gel (240 g) column chromatography using MeOH--CHCl3 (1:10) as an eluent to give 5.23 g of an orange-colored oil. To this oil were added small amounts of EtOH and ether and the mixture was cooled in a dry ice-acetone bath and triturated to give crystals. After addition of ether, the crystals were collected by filtration, washed with ether and dried. The procedure gave 3.69 g of the title compound as pale yellow cyrstals.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. temperaturethe mixture was refluxed for 6.5 hours
  2. distillationThe nitromethane was distilled off

出典と根拠

ORDレコード
ord-4a00f573b92c47dd8b3670ac44ff43a1
出典データセット
uspto-grants-2000_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06124297

反応ノート

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