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2-Methyl-2-butanol → 2-Amino-4-methoxy-5-(3-morpholinopropoxy)benzamide

HRID 646535
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HRID 646535 반응식
[NH2:1][C:2]1[CH:9]=[C:8]([O:10][CH3:11])[C:7]([O:12][CH2:13][CH2:14][CH2:15][N:16]2[CH2:21][CH2:20][O:19][CH2:18][CH2:17]2)=[CH:6][C:3]=1[C:4]#[N:5].C([OH:27])(CC)(C)C>C(Cl)Cl>[NH2:1][C:2]1[CH:9]=[C:8]([O:10][CH3:11])[C:7]([O:12][CH2:13][CH2:14][CH2:15][N:16]2[CH2:17][CH2:18][O:19][CH2:20][CH2:21]2)=[CH:6][C:3]=1[C:4]([NH2:5])=[O:27]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 64052-Methyl-2-butanolHCID 100628722-Amino-4-methoxy-5-(3-morpholinopropoxy)benzonitrile

생성물 1

HCID 116381442-Amino-4-methoxy-5-(3-morpholinopropoxy)benzamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
79 °C

실험 절차

After repetition of the reduction step, a methylene chloride solution (894.3 kg) containing 2-amino-4-methoxy-5-(3-morpholinopropoxy)benzonitrile (81.6 kg) was added portionwise to tert-amyl alcohol (186 kg) and the resultant mixture was distilled until the temperature of the distillate reached 57° C. Additional tert-amyl alcohol (726 kg) was added portionwise and distillation was continued until the residual volume of the reaction mixture was approximately 770 liters. Potassium hydroxide (flaked form; 51 kg) was added and the mixture was heated to 79° C. for 4 hours. The resultant mixture was cooled to ambient temperature to provide a solution of 2-amino-4-methoxy-5-(3-morpholinopropoxy)benzamide which was used without being isolated.

후처리

  1. distillationthe resultant mixture was distilled until the temperature of the distillate
  2. customreached 57° C
  3. additionAdditional tert-amyl alcohol (726 kg) was added portionwise
  4. distillationdistillation
  5. additionPotassium hydroxide (flaked form; 51 kg) was added
  6. temperatureThe resultant mixture was cooled to ambient temperature

출처 및 근거

ORD 기록
ord-922d6e2e4fb5489c9676dcc6d8e4e890
출처 데이터셋
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07705145B2

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