Guanidine Hydrochloride → HCID 18945440、化合物

HRID 399870ノート

反応式

HRID 399870 の反応式
[I-].ClC1C=CC=C[N+]=1C.[C:10]([C:12]1[CH:13]=[C:14]([N:21]2[CH:25]=[CH:24][CH:23]=[CH:22]2)[CH:15]=[C:16]([CH:20]=1)[C:17]([OH:19])=O)#[N:11].Cl.[NH2:27][C:28]([NH2:30])=[NH:29].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O.O.O1CCCC1.C(OCC)(=O)C.C(N(CC)CC)C>[C:10]([C:12]1[CH:13]=[C:14]([N:21]2[CH:25]=[CH:24][CH:23]=[CH:22]2)[CH:15]=[C:16]([CH:20]=1)[C:17]([N:27]=[C:28]([NH2:30])[NH2:29])=[O:19])#[N:11]

参加物

10

反応物 4

HCID 5742Guanidine HydrochlorideHCID 11430Potassium CarbonateHCID 1670692-Chloro-1-methylpyridinium iodideHCID 18945142HCID 18945142、化合物

生成物 1

HCID 18945440HCID 18945440、化合物収率 62.4%

試薬・触媒・溶媒 5

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8028Tetrahydrofuran溶媒HCID 8471Triethylamine溶媒HCID 8857Ethyl Acetate溶媒

実験手順

2-Chloro-1-methylpyridinium iodide (3.6 g) was added to a mixture of 5-cyano-3-(pyrrol-1-yl)benzoic acid (2.0 g), guanidine hydrochloride (2.7 g) and triethylamine (7.2 ml) in N,N-dimethylformamide (30 ml), and the mixture was stirred for 4 hours at ambient temperature. The reaction mixture was added to a mixture of ethyl acetate, tetrahydrofuran and water, and adjusted to pH 10 with potassium carbonate. The separated organic layer was washed with brine and dried over magnesium sulfate. The solvent was removed by concentration and the residue was triturated with ether to give 2-[5-cyano-3-(pyrrol-1-yl)benzoyl]guanidine (1.49 g).

後処理

  1. washThe separated organic layer was washed with brine
  2. dry with materialdried over magnesium sulfate
  3. customThe solvent was removed by concentration
  4. customthe residue was triturated with ether

出典と根拠

ORDレコード
ord-156620907c0947a4aac9e70f4121b764
出典データセット
uspto-grants-1998_10
特許番号
US05824691

反応ノート

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