Acetic Acid → HCID 178476708、化合物

HRID 556735ノート

反応式

HRID 556735 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]1[CH:12]=[CH:11][CH:10]=[C:9]1[CH:13]=[CH:14][CH:15]=O.C(=O)(O)O.[NH2:21][NH:22][C:23]([NH2:25])=[NH:24].[C:26]([OH:29])(=[O:28])[CH3:27]>C(O)C>[C:26]([O-:29])(=[O:28])[CH3:27].[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]1[CH:12]=[CH:11][CH:10]=[C:9]1[CH:13]=[CH:14][CH:15]=[N:21][NH:22][C:23]([NH2:25])=[NH2+:24]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 86652392HCID 86652392、化合物HCID 178513185HCID 178513185、化合物

生成物 1

HCID 178476708HCID 178476708、化合物収率 31%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

0.9 g (3.26 mmol) 4b and 1.2 eqv. of aminoguanidine bicarbonate was mixed in 10 ml of ethanol and 2 ml of acetic acid and refluxed for 30 min. The solvent was evaporated and the oily residue was dissolved in acetonitrile and a few drops of diethyl ether was added. After three days in refrigerator a precipitate was formed that was filtered, washed with diethyl ether and dried. 340 mg (31%) of the final product 5b was obtained as white crystals (m.p. 166-168° C.).

後処理

  1. customThe solvent was evaporated
  2. dissolutionthe oily residue was dissolved in acetonitrile
  3. additiona few drops of diethyl ether was added
  4. customAfter three days in refrigerator a precipitate was formed
  5. filtrationthat was filtered
  6. washwashed with diethyl ether
  7. customdried

出典と根拠

ORDレコード
ord-296e9030752d4fcbbb67d3f09bf32613
出典データセット
uspto-grants-2011_11
特許番号
US08058306B2

反応ノート

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