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Carbamic acid, ethyl ester → Ethyl di(4-docosoxyphenyl)methylcarbamate

HRID 1754831
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HRID 1754831 반응식
[CH2:1]([O:23][C:24]1[CH:29]=[CH:28][C:27]([CH:30]([C:32]2[CH:37]=[CH:36][C:35]([O:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH2:46][CH2:47][CH2:48][CH2:49][CH2:50][CH2:51][CH2:52][CH2:53][CH2:54][CH2:55][CH2:56][CH2:57][CH2:58][CH2:59][CH3:60])=[CH:34][CH:33]=2)O)=[CH:26][CH:25]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH3:22].[C:61](=[O:66])([O:63][CH2:64][CH3:65])[NH2:62].CS(O)(=O)=O.C(=O)([O-])[O-].[Na+].[Na+]>C1(C)C=CC=CC=1>[CH2:1]([O:23][C:24]1[CH:29]=[CH:28][C:27]([CH:30]([NH:62][C:61](=[O:66])[O:63][CH2:64][CH3:65])[C:32]2[CH:37]=[CH:36][C:35]([O:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH2:46][CH2:47][CH2:48][CH2:49][CH2:50][CH2:51][CH2:52][CH2:53][CH2:54][CH2:55][CH2:56][CH2:57][CH2:58][CH2:59][CH3:60])=[CH:34][CH:33]=2)=[CH:26][CH:25]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH3:22]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 5641Carbamic acid, ethyl esterHCID 6395Methanesulfonic Acid2회HCID 10340Sodium CarbonateHCID 469361424,4'-Didocosoxybenzhydrol

생성물 1

HCID 86646200Ethyl di(4-docosoxyphenyl)methylcarbamate수율 103.8%

시약·촉매·용매 1

HCID 1140
Toluene
용매

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온도
110 °C

실험 절차

To bis-(4-docosoxy-phenyl)-methanol (28.5 g, 34.2 mmol) were added toluene (350 mL), ethyl carbamate (6.1 g, 68.5 mmol) and methanesulfonic acid (333 μL, 5.14 mmol) and the mixture was stirred at 110° C. for 2 hr. Methanesulfonic acid (333 μL, 5.14 mmol) was added and the mixture was stirred for 30 min. After stirring, the reaction mixture was cooled to room temperature, sodium carbonate (1.1 g, 8.73 mmol) was added and the solvent was evaporated. The residue was crystallized from methanol (400 mL) to give ethyl [bis-(4-docosoxy-phenyl)-methyl]carbamate (32.1 g, 100%).

후처리

  1. stirringthe mixture was stirred for 30 min
  2. stirringAfter stirring
  3. temperaturethe reaction mixture was cooled to room temperature
  4. customthe solvent was evaporated
  5. customThe residue was crystallized from methanol (400 mL)

출처 및 근거

ORD 기록
ord-422955909eb347c9898297df40566305
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09169187B2

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