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Ammonia → HCID 21504501、化合物

HRID 1288273
ノート
印刷プレビュー

反応式

HRID 1288273 の反応式
[CH3:1][O:2][C:3]1[C:13]([CH3:14])=[CH:12][CH:11]=[CH:10][C:4]=1[C:5](=[NH:9])OCC.[NH3:15].[ClH:16]>C(O)C.C(OCC)C>[ClH:16].[CH3:1][O:2][C:3]1[C:13]([CH3:14])=[CH:12][CH:11]=[CH:10][C:4]=1[C:5]([NH2:9])=[NH:15]
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 3

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 21504428HCID 21504428、化合物

生成物 1

HCID 21504501HCID 21504501、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒2 回HCID 3283Diethyl Ether溶媒2 回

実験手順

Ethyl 2-methoxy-3-methylbenzimidate borofluoride (28 g.) was mixed with a saturated anhydrous solution of ammonia in ethanol (46 ml.), the mixture was kept at room temperature in a stoppered vessel for 3 days and then evaporated to dryness in vacuo. The residue was dissolved in water (25 ml.) and treated with 5N sodium hydroxide solution (50 ml.). The solution was saturated with sodium chloride and extracted with diethyl ether. The extract was dried over potassium hydroxide and evaporated to give crude 2-methoxy-3-methylbenzamidine, m.p. 72°-74° C. This was dissolved in anhydrous ethanol (40 ml.) and the solution treated with a saturated anhydrous solution of hydrogen chloride in diethyl ether (100 ml.), and diluted with anhydrous diethyl ether (100 ml.). The solid which separated was filtered off and washed with anhydrous diethyl ether to give 2-methoxy-3-methylbenzamidine hydrochloride (17.8 g.), m.p. 208°-209° C. (with decomposition).

後処理

  1. customevaporated to dryness in vacuo
  2. dissolutionThe residue was dissolved in water (25 ml.)
  3. additiontreated with 5N sodium hydroxide solution (50 ml.)
  4. extractionextracted with diethyl ether
  5. dry with materialThe extract was dried over potassium hydroxide
  6. customevaporated
  7. customto give crude 2-methoxy-3-methylbenzamidine, m.p. 72°-74° C
  8. customThe solid which separated
  9. filtrationwas filtered off
  10. washwashed with anhydrous diethyl ether

出典と根拠

ORDレコード
ord-cd9a99b1730f4009b48728828ad88cf7
出典データセット
uspto-grants-1976_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03987160

反応ノート

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