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Dichloromethane → N-(4-methoxybenzyl)-1H-imidazole-1-carboxamide

HRID 1589788
ノート
印刷プレビュー

反応式

HRID 1589788 の反応式
[C:1]([N:8]1[CH:12]=[CH:11]N=C1)([N:3]1[CH:7]=[CH:6][N:5]=[CH:4]1)=[O:2].[CH3:13][O:14][C:15]1[CH:22]=[CH:21]C(CN)=[CH:17][CH:16]=1.C(Cl)Cl>O1CCCC1>[CH3:13][O:14][C:15]1[CH:22]=[CH:21][C:11]([CH2:12][NH:8][C:1]([N:3]2[CH:7]=[CH:6][N:5]=[CH:4]2)=[O:2])=[CH:17][CH:16]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6344DichloromethaneHCID 682631,1'-CarbonyldiimidazoleHCID 754524-Methoxybenzylamine

生成物 1

HCID 9991495N-(4-methoxybenzyl)-1H-imidazole-1-carboxamide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

23.6 g of carbonyldiimidazole are added in portions to a solution of 20 g of 4-methoxybenzylamine in 100 ml of anhydrous tetrahydrofuran, the temperature being kept below 10° C. When the addition is complete, the mixture is allowed to return to room temperature and stirring is maintained for three hours. After filtration, the tetrahydrofuran phase is evaporated under vacuum and the residue obtained is taken up with methylene chloride, washed with water and then dried. The oil obtained after evaporation of the methylene chloride is crystallized from ether. The crystals obtained are filtered off and then dried. 22.7 g of N-(4-methoxybenzyl)imidazolecarboxamide are thus recovered in the form of crystals melting at 117° C.

後処理

  1. custombeing kept below 10° C
  2. additionWhen the addition
  3. customto return to room temperature
  4. temperatureis maintained for three hours
  5. filtrationAfter filtration
  6. customthe tetrahydrofuran phase is evaporated under vacuum
  7. customthe residue obtained
  8. washwashed with water
  9. customdried
  10. customThe oil obtained
  11. customafter evaporation of the methylene chloride
  12. customis crystallized from ether
  13. customThe crystals obtained
  14. filtrationare filtered off
  15. customdried
  16. custom22.7 g of N-(4-methoxybenzyl)imidazolecarboxamide are thus recovered in the form of crystals melting at 117° C.

出典と根拠

ORDレコード
ord-e9904591839841c786e9ef790ee46afc
出典データセット
uspto-grants-1993_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05200408

反応ノート

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