Methanol → HCID 15782683, 화합물

HRID 992159

반응식

HRID 992159 반응식
[C:1](Cl)(=O)C.C(N(CC)CC)C.CO.[C:14]([C:17]12[CH2:26][CH:21]3[CH2:22][CH:23]([CH2:25][C:19]([N+:27]([O-:29])=[O:28])([CH2:20]3)[CH2:18]1)[CH2:24]2)([OH:16])=[O:15]>CN(C=O)C>[CH3:1][O:15][C:14]([C:17]12[CH2:26][CH:21]3[CH2:22][CH:23]([CH2:25][C:19]([N+:27]([O-:29])=[O:28])([CH2:20]3)[CH2:18]1)[CH2:24]2)=[O:16]

참가 물질

6

반응물 4

HCID 887MethanolHCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 392393-Nitrotricyclo(3.3.1.13,7)decane-1-carboxylic acid

생성물 1

HCID 15782683HCID 15782683, 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 42 was dissolved in 10ml 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, 20 mmole of triethylamine was added, and then 11 mmole of methanol 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-methoxycarbonyl-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. temperaturethe mixture was cooled
  5. customat 10° C. or less

출처 및 근거

ORD 기록
ord-2797b2fbc30c4e2f9176f399c466e35e
출처 데이터셋
uspto-grants-2002_10
특허 번호
US06468487B1

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