Toluene → HCID 178517902, 화합물

HRID 2072474노트

반응식

HRID 2072474 반응식
[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3][C:2]=1[CH2:11][N:12]1[CH2:20][CH2:19][C:15]([NH:21][C:22]2C=CC=CC=2)([C:16]([NH2:18])=[O:17])[CH2:14][CH2:13]1.C(OCC)(OCC)OCC.C1(C)C=CC=CC=1.[OH-].[NH4+]>C(O)(=O)C>[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3][C:2]=1[CH2:11][N:12]1[CH2:13][CH2:14][C:15]2([NH:21][CH:22]=[N:18][C:16]2=[O:17])[CH2:19][CH2:20]1

참가 물질

6

반응물 4

HCID 1140TolueneHCID 14923Ammonium HydroxideHCID 31214Ethyl orthoformateHCID 214082231-[(3,4-Dihydro-2-naphthalenyl)methyl]-4-anilino isonipecotamide

생성물 1

HCID 178517902HCID 178517902, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A mixture of 1-[(3,4-dihydro-2-naphthalenyl)methyl]-4-anilino isonipecotamide (6.0 g), triethyl orthoformate (3.0 g), toluene (30 ml), and glacial acetic acid (1.5 ml) is refluxed under nitrogen for 38 hours. The reaction mixture is cooled and poured into aqueous ammonium hydroxide. The organic layer is separated, dried, and concentrated to give the crude product. Digestion of this material with benzene followed by filtration and concentration of the organic solution yields the title compound.

후처리

  1. temperatureis refluxed under nitrogen for 38 hours
  2. temperatureThe reaction mixture is cooled
  3. customThe organic layer is separated
  4. customdried
  5. concentrationconcentrated
  6. customto give the crude product
  7. filtrationDigestion of this material with benzene followed by filtration and concentration of the organic solution

출처 및 근거

ORD 기록
ord-ef88f300af0b4791a2a6a5332dce9a59
출처 데이터셋
uspto-grants-1977_09
특허 번호
US04051248

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