Potassium Carbonate → HCID 59591441, 화합물

HRID 1963000노트

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HRID 1963000 반응식
[F:1][C:2]1[C:7]([OH:8])=[CH:6][CH:5]=[C:4]([F:9])[C:3]=1[C:10]#[N:11].C([O-])([O-])=O.[K+].[K+].N[C@H](C(O)=O)CC1C=C2C(C=CC=C2)=CC=1.[Cl:34][C:35]1[CH:36]=[CH:37][C:38]2[S:42][C:41]([CH2:43]Cl)=[N:40][C:39]=2[CH:45]=1>CN(C=O)C.O>[Cl:34][C:35]1[CH:36]=[CH:37][C:38]2[S:42][C:41]([CH2:43][O:8][C:7]3[C:2]([F:1])=[C:3]([C:10]#[N:11])[C:4]([F:9])=[CH:5][CH:6]=3)=[N:40][C:39]=2[CH:45]=1

참가 물질

7

반응물 4

HCID 11430Potassium CarbonateHCID 1859152-NaphthylalanineHCID 107988395-Chloro-2-(chloromethyl)-1,3-benzothiazoleHCID 451191012,6-Difluoro-3-hydroxybenzonitrile

생성물 1

HCID 59591441HCID 59591441, 화합물수율 79%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

A mixture of 2,6-difluoro-3-hydroxybenzenecarbonitrile (4.5 g, 29.0 mmol), K2CO3 (6.01 g, 43.5 mmol) and Nal (0.78 g 5.8 mmol) in DMF (75 ml) was stirred at room temperature for 5 minutes. 5-chloro-2-(chloromethyl)-1,3-benzothiazole was then added and the mixture heated at 40° C. for 18 hours, cooled to room temperature and poured into water (450 ml). Buff solid was filtered off and dried (9.46 g). This was the recrystallised from acetonitrile (30 ml) and dried in vacuo at 40° C. to give a beige solid. Yield 79%, mp 145-147° C., HPLC (Gemini C18, 50×4.6 mm): m/z 337 [M+H]+, Rt=4.93 min.

후처리

  1. temperaturethe mixture heated at 40° C. for 18 hours
  2. temperaturecooled to room temperature
  3. filtrationBuff solid was filtered off
  4. customdried (9.46 g)
  5. customrecrystallised from acetonitrile (30 ml)
  6. customdried in vacuo at 40° C.
  7. customto give a beige solid

출처 및 근거

ORD 기록
ord-057c172684ac495987a9fc0f6c25c561
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08415383B2

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