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HCID 22450431, 화합물 → N-methyl-1-(pyridin-2-yl)methanamine

HRID 1457903
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반응식

HRID 1457903 반응식
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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 22450431HCID 22450431, 화합물HCID 22450450HCID 22450450, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 6375Nitromethane용매

실험 절차

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 crystals.

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후처리

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

출처 및 근거

ORD 기록
ord-9f14653525b34925b578bce1f81e4ec2
출처 데이터셋
uspto-grants-1998_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05849768

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