Dimethylformamide → Benzamide

HRID 280336

反応式

HRID 280336 の反応式
N1[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[C:4](=O)[O:3]C1=O.C[N:14](C)C=O.NCCN1CCC(NC2N(CC3C=CC(F)=CC=3)C3C=CC=CC=3N=2)CC1>O>[C:4]([NH2:14])(=[O:3])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1

参加物

5

反応物 3

HCID 6228Dimethylformamide2 回HCID 8359Isatoic AnhydrideHCID 12891741N-[1-(2-aminoethyl)-4-piperidinyl]-1-(4-fluorophenylmethyl)-1H-benzimidazol-2-amine

生成物 1

HCID 2331Benzamide

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a stirred and hot (50° C.) mixture of 4.1 parts of 2H-3,1-benzoxazine-2,4(1H)-dione and 31.5 parts of N,N-dimethylformamide was added dropwise a solution of 9.4 parts of N-[1-(2-aminoethyl)-4-piperidinyl]-1-[(4-fluorophenyl)methyl]-1H-benzimidazol-2-amine in 31.5 parts of N,N-dimethylformamide at 50° C. Upon completion, stirring was continued for 3 hours at 50° C. Water was added and the product was extracted with 4-methyl-2- pentanone. The extract was dried, filtered and evaporated. The residue was crystallized from acetonitrile, yielding 9.8 parts (80%) of 2-amino-N-[2-[4-fluorophenyl)-methyl]-1H-benzimidazol-2-yl]amino]-1-piperidinyl]ethyl]benzamide; mp. 171.7° C. (58).

後処理

  1. stirringUpon completion, stirring
  2. extractionthe product was extracted with 4-methyl-2- pentanone
  3. customThe extract was dried
  4. filtrationfiltered
  5. customevaporated
  6. customThe residue was crystallized from acetonitrile

出典と根拠

ORDレコード
ord-ff3957c71daa4453bbb438ca724371dc
出典データセット
uspto-grants-1986_05
特許番号
US04588722

関連ノート

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