Acetic Acid → 3,4-Dichloro-5-methyl-N-(1-nitrosopiperidin-4-yl)-1H-pyrrole-2-carboxamide

HRID 2233874노트

반응식

HRID 2233874 반응식
[N:1]([O-:3])=O.[Na+].FC(F)(F)C([O-])=O.[Cl:12][C:13]1[C:17]([Cl:18])=[C:16]([CH3:19])[NH:15][C:14]=1[C:20]([NH:22][CH:23]1[CH2:28][CH2:27][NH2+:26][CH2:25][CH2:24]1)=[O:21].C(O)(=O)C>O.C(O)C.O>[Cl:12][C:13]1[C:17]([Cl:18])=[C:16]([CH3:19])[NH:15][C:14]=1[C:20]([NH:22][CH:23]1[CH2:28][CH2:27][N:26]([N:1]=[O:3])[CH2:25][CH2:24]1)=[O:21]

참가 물질

6

반응물 3

HCID 176Acetic AcidHCID 23668193Sodium NitriteHCID 685798674-{[(3,4-Dichloro-5-methyl-1H-pyrrol-2-yl)carbonyl]amino}piperidinium trifluoroacetate2회

생성물 1

HCID 866082583,4-Dichloro-5-methyl-N-(1-nitrosopiperidin-4-yl)-1H-pyrrole-2-carboxamide

시약·촉매·용매 2

HCID 962Water용매2회HCID 19096565Water ethanol용매

반응 조건

온도
90 °C

실험 절차

A solution of NaNO2 (1.7 g, 24.6 mmol) in 20 ml of water was added to a solution of 4-{[(3,4-dichloro-5-methyl-1H-pyrrol-2-yl)carbonyl]amino}piperidinium trifluoroacetate (Intermediate 86; 4 g, 10.3 mmol) and 400 μl acetic acid in 60 ml of 1:1 EtOH—H2O. The mixture was heated to 90° C. for 1 hour. After cooling to room temperature, 200 ml of water was added. White solids were collected by filtration and dried in vacuo (2.8 g).

후처리

  1. temperatureAfter cooling to room temperature
  2. filtrationWhite solids were collected by filtration
  3. customdried in vacuo (2.8 g)

출처 및 근거

ORD 기록
ord-df58e45c1d7c497faec733b0e8249d0d
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07709503B2

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