Guanidine Hydrochloride → HCID 18945440, 화합물

HRID 399870노트

반응식

HRID 399870 반응식
[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]

참가 물질

10

반응물 4

HCID 5742Guanidine HydrochlorideHCID 11430Potassium CarbonateHCID 1670692-Chloro-1-methylpyridinium iodideHCID 18945142HCID 18945142, 화합물

생성물 1

HCID 18945440HCID 18945440, 화합물수율 62.4%

시약·촉매·용매 5

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 8028Tetrahydrofuran용매HCID 8471Triethylamine용매HCID 8857Ethyl Acetate용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-156620907c0947a4aac9e70f4121b764
출처 데이터셋
uspto-grants-1998_10
특허 번호
US05824691

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