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

HRID 1585035
ノート
印刷プレビュー

反応式

HRID 1585035 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-chloro-benzyl)-N-methyl-N'-methylisothiourea prepared in (1) was added 25 ml of nitromethane and the mixture was reflexed 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 crystals.

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. distillationThe nitromethane was distilled off

出典と根拠

ORDレコード
ord-2729e782010441ff9c0e3375d4b634f1
出典データセット
uspto-grants-1999_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05935981

反応ノート

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