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Ammonia → HCID 13056027, 화합물

HRID 2198757
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HRID 2198757 반응식
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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

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

생성물 1

HCID 13056027HCID 13056027, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-877f600815624a71bee134eec044f646
출처 데이터셋
uspto-grants-1982_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04359468

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