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Ammonia → HCID 13056027、化合物

HRID 2198757
ノート
印刷プレビュー

反応式

HRID 2198757 の反応式
O=[C:2]1[CH2:7][CH2:6][N:5]([CH2:8][CH2:9][CH2:10][N:11]2[C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=3[NH:13][C:12]2=[O:20])[CH2:4][CH2:3]1.[CH3:21][N:22]1[C:30]2[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=2)[CH:24]=[CH:23]1.P(=O)(O)(O)O.N>C(O)(=O)C>[CH3:21][N:22]1[C:30]2[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=2)[C:24]([CH:2]2[CH2:7][CH2:6][N:5]([CH2:8][CH2:9][CH2:10][N:11]3[C:15]4[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=4[NH:13][C:12]3=[O:20])[CH2:4][CH2:3]2)=[CH:23]1
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 4

HCID 222AmmoniaHCID 1004Phosphoric AcidHCID 117811-MethylindoleHCID 13056043N-[3-(4-oxo-piperidino)-propyl]-benzimidazolone

生成物 1

HCID 13056027HCID 13056027、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A mixture consisting of 2.7 gm of N-[3-(4-oxo-piperidino)-propyl]-benzimidazolone, 1.3 gm of 1-methylindole, 40 ml of acetic acid and 10 ml of 2 N phosphoric acid was allowed to stand at 20° C. for 6 days. Thereafter, the reaction mixture was poured into a mixture of ice and ammonia, the aqueous mixture was extracted with ethyl acetate, and the extract solution was dried and evaporated in vacuo to dryness. The residue was purified by chromatography on silica, using methylene chloride/methanol/ammonia=90/9/1 as the eluant. The main fraction was hydrogenated without characterization as described in Example 1, and the end product was crystallized from ethanol, yielding 2.4 gm (62% of theory) of the compound of the formula ##STR14## having a melting point of 180° C.

後処理

  1. extractionthe aqueous mixture was extracted with ethyl acetate
  2. customthe extract solution was dried
  3. customevaporated in vacuo to dryness
  4. customThe residue was purified by chromatography on silica
  5. customthe end product was crystallized from ethanol
  6. customyielding 2.4 gm (62% of theory) of the compound of the formula

出典と根拠

ORDレコード
ord-877f600815624a71bee134eec044f646
出典データセット
uspto-grants-1982_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04359468

反応ノート

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