Dimethylamine → HCID 18410501, 화합물

HRID 992160

반응식

HRID 992160 반응식
C(Cl)(=O)C.[CH3:5][NH:6][CH3:7].[C:8]([C:11]12[CH2:20][CH:15]3[CH2:16][CH:17]([CH2:19][C:13]([N+:21]([O-:23])=[O:22])([CH2:14]3)[CH2:12]1)[CH2:18]2)(O)=[O:9]>CN(C=O)C>[CH3:5][N:6]([CH3:7])[C:8]([C:11]12[CH2:20][CH:15]3[CH2:16][CH:17]([CH2:19][C:13]([N+:21]([O-:23])=[O:22])([CH2:14]3)[CH2:12]1)[CH2:18]2)=[O:9]

참가 물질

5

반응물 3

HCID 674DimethylamineHCID 6367Acetyl chlorideHCID 392393-Nitrotricyclo(3.3.1.13,7)decane-1-carboxylic acid

생성물 1

HCID 18410501HCID 18410501, 화합물수율 95%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

In an atmosphere of nitrogen, 10 mmole of 1-carboxy-3-nitroadamantane obtained by the method of Example 43 was dissolved in 10 ml of DMF. To the mixture, 15 mmole of acetyl chloride was added dropwise over 30 minutes. The mixture was heated to begin to reflux around the conclusion of the addition. After refluxing for 2 hours, the mixture was cooled,and 25 mmole of dimethylamine was added dropwise over 30 minutes while retaining the temperature of the mixture at 10° C. or less followed by stirring for more 2 hours. As a result, the conversion of 1-carboxy-3-nitroadamantane was 99%, and 1-(N,N-dimethylcarbamoyl)-3-nitroadamantane (yield 95%) was formed.

후처리

  1. temperatureThe mixture was heated
  2. temperatureto reflux around the conclusion of the addition
  3. temperatureAfter refluxing for 2 hours
  4. additionwas added dropwise over 30 minutes
  5. customat 10° C. or less

출처 및 근거

ORD 기록
ord-01f4e1c48de94dbfac23ea147987f5e6
출처 데이터셋
uspto-grants-2002_10
특허 번호
US06468487B1

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