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Ethanol → DW-1350

HRID 732248
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HRID 732248 반응식
[CH:1]([C:4]1[S:8][C:7]([CH3:9])=[N:6][C:5]=1[C:10]1[CH:30]=[CH:29][C:13]([O:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][O:20][C:21]2[CH:28]=[CH:27][C:24]([C:25]#[N:26])=[CH:23][CH:22]=2)=[CH:12][CH:11]=1)([CH3:3])[CH3:2].C(O)C.Cl.[NH2:35][OH:36].C(N(CC)CC)C>O>[OH:36][NH:35][C:25](=[NH:26])[C:24]1[CH:23]=[CH:22][C:21]([O:20][CH2:19][CH2:18][CH2:17][CH2:16][CH2:15][O:14][C:13]2[CH:29]=[CH:30][C:10]([C:5]3[N:6]=[C:7]([CH3:9])[S:8][C:4]=3[CH:1]([CH3:2])[CH3:3])=[CH:11][CH:12]=2)=[CH:28][CH:27]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 702EthanolHCID 8471TriethylamineHCID 443297Hydroxyamine hydrochlorideHCID 162024464-{5-[4-(5-Isopropyl-2-Methyl-1,3-Thiazol-4-Yl)-Phenoxy]-Pentoxy}-Benzonitrile

생성물 1

HCID 178432563DW-1350수율 95%

시약·촉매·용매 1

HCID 962Water
용매

실험 절차

While 45 g of 4-5-[4-(5-isopropyl-2-methyl-1,3-thiazol-4-yl)-phenoxy]-pentoxy-benzonitrile (10) prepared in Example 6 were added to 300 ml of ethanol and stirred, 15 g of hydroxylamine hydrochloride and 30 ml of triethylamine were added. The temperature was gradually increased and stirring under reflux was continued for 15 hr. After the reaction was completed, the temperature was decreased to 40° C., and the resultant reaction solution was slowly added with water, thereby being crystallized. The precipitated solid was filtered and washed with water, thus obtaining 44.2 g (yield: 95%) of a title compound as a white solid.

후처리

  1. temperatureThe temperature was gradually increased
  2. stirringstirring
  3. temperatureunder reflux
  4. customwas decreased to 40° C.
  5. customthe resultant reaction solution
  6. custombeing crystallized
  7. filtrationThe precipitated solid was filtered
  8. washwashed with water

출처 및 근거

ORD 기록
ord-1399806e59e64f8f8ec64ab6507d2a36
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07585979B2

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