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Hydrochloric Acid → Methyl (4,6-dimethoxy-1,3,5-triazin-2-yl)carbamate

HRID 542683
ノート
印刷プレビュー

反応式

HRID 542683 の反応式
[NH2:1][C:2]1[N:7]=[C:6]([O:8][CH3:9])[N:5]=[C:4]([O:10][CH3:11])[N:3]=1.[H-].[Na+].[CH3:14][O:15][C:16](=O)[O:17]C.Cl>O1CCCC1>[CH3:9][O:8][C:6]1[N:5]=[C:4]([O:10][CH3:11])[N:3]=[C:2]([NH:1][C:16](=[O:17])[O:15][CH3:14])[N:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 12021Dimethyl CarbonateHCID 24758Sodium hydrideHCID 278402-Amino-4,6-dimethoxy-1,3,5-triazine

生成物 1

HCID 12803256Methyl (4,6-dimethoxy-1,3,5-triazin-2-yl)carbamate収率 57.9%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran
溶媒
2 回

実験手順

2-Amino-4,6-dimethoxy-1,3,5-triazine (55.3 g) was added portionwise to 50% sodium hydride (38.0 g) in 1000 ml dry tetrahydrofuran at ambient temperature under nitrogen. After the reaction mixture was stirred for 1.25 hours, dimethylcarbonate (50.0 g) was added dropwise. The reaction mixture was stirred 16 hours at ambient temperature under nitrogen and concentrated hydrochloric acid (68 ml) was slowly added followed by 100 ml tetrahydrofuran. Insoluble material was removed via filtration and discarded. The filtrate was dried and the solvent removed under reduced pressure to give a solid which upon crystallization from ethanol afforded 43.9 g of the tital compound, m.p. 118°-122° C.

後処理

  1. stirringThe reaction mixture was stirred 16 hours at ambient temperature under nitrogen
  2. customInsoluble material was removed via filtration
  3. customThe filtrate was dried
  4. customthe solvent removed under reduced pressure
  5. customto give a solid which
  6. customupon crystallization from ethanol

出典と根拠

ORDレコード
ord-d5243c0a63c7401981cd15cdf632fc53
出典データセット
uspto-grants-1987_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04659368

反応ノート

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