Hydrochloric Acid → Roflumilast

HRID 42680

반응식

HRID 42680 반응식
[K].[NH2:2][C:3]1[C:8]([Cl:9])=[CH:7][N:6]=[CH:5][C:4]=1[Cl:10].[CH:11]1([CH2:14][O:15][C:16]2[CH:17]=[C:18]([CH:22]=[CH:23][C:24]=2[O:25][CH:26]([F:28])[F:27])[C:19](Cl)=[O:20])[CH2:13][CH2:12]1.Cl>CN(C=O)C.O>[CH:22]1[C:18]([C:19]([NH:2][C:3]2[C:4]([Cl:10])=[CH:5][N:6]=[CH:7][C:8]=2[Cl:9])=[O:20])=[CH:17][C:16]([O:15][CH2:14][CH:11]2[CH2:12][CH2:13]2)=[C:24]([O:25][CH:26]([F:27])[F:28])[CH:23]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 898884-Amino-3,5-dichloropyridineHCID 5462222PotassiumHCID 120473303-(Cyclopropylmethoxy)-4-(difluoromethoxy)benzoyl chloride

생성물 1

HCID 449193Roflumilast

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매2회

반응 조건

온도
25 °C

실험 절차

The potassium salt suspension of the anion of 4-amino-3,5-dichloropyridine in DMF (2-2.5 equivalents) is introduced into a reaction vessel. A solution of 3-cyclopropylmethoxy-4-difluoromethoxybenzoyl chloride (1 equivalent) in DMF is slowly added to this suspension while stirring vigorously at a temperature of 15 to 40° C., preferably 20 to 30° C. After the reaction is complete, water is slowly added while stirring at 15-25° C., and the pH is adjusted to 2-3 with hydrochloric acid.

후처리

  1. additionis introduced into a reaction vessel
  2. stirringwhile stirring at 15-25° C.

출처 및 근거

ORD 기록
ord-cd988c3896aa452ba5e90738334d9fe9
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08536206B2

연결된 노트

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