Hydrogen Bromide → HCID 136131615, 화합물

HRID 911204노트

반응식

HRID 911204 반응식
Br.[CH2:2]([C:4]1[CH:9]=[C:8]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[N:7]=[N:6][C:5]=1[NH:16][C:17]1[CH:22]=[CH:21][C:20]([O:23]C)=[CH:19][CH:18]=1)[CH3:3].C([O-])([O-])=O.[Na+].[Na+]>CC(O)=O>[CH2:2]([C:4]1[CH:9]=[C:8]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[N:7]=[N:6][C:5]=1[NH:16][C:17]1[CH:18]=[CH:19][C:20]([OH:23])=[CH:21][CH:22]=1)[CH3:3]

참가 물질

5

반응물 3

HCID 260Hydrogen BromideHCID 10340Sodium CarbonateHCID 57756259HCID 57756259, 화합물

생성물 1

HCID 136131615HCID 136131615, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
140 °C

실험 절차

A RBF was charged with 13.9 mL of 1:1 AcOH:HBr and 4-ethyl-N-(4-methoxyphenyl)-6-phenylpyridazin-3-amine (1.27 g, 4.16 mmol). The flask was fitted with a reflux condenser and was heated at 140° C. for 4 h. Upon cooling, the reaction mixture was poured into ice water and brought to neutral pH by careful addition of 2M aqueous Na2CO3. The resulting precipitate was filtered, washed with water and dried under vacuum to provide 4-(4-ethyl-6-phenylpyridazin-3-ylamino)phenol as a tan solid. MS m/z=292 [M+H]+. Calc'd for C18H17N3O: 291.35.

후처리

  1. customThe flask was fitted with a reflux condenser
  2. temperatureUpon cooling
  3. filtrationThe resulting precipitate was filtered
  4. washwashed with water
  5. customdried under vacuum

출처 및 근거

ORD 기록
ord-e0f90fa98a1f4748b34226e0a1279699
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08022221B2

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