홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Ammonium Chloride → HCID 23156849, 화합물

HRID 1098297
노트
인쇄 미리보기

반응식

HRID 1098297 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH3:13])=[C:6]([CH:12]=1)[C:7]([N:9]([CH3:11])C)=[O:8].[CH2:14]1[N:19]([C:20]2[C:25](C#N)=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH2:18][CH2:17][O:16][CH2:15]1.[Cl-].[NH4+]>C1COCC1>[Cl:1][C:2]1[CH:12]=[C:6]2[C:5]([CH:13]=[C:11]([C:21]3[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=3[N:19]3[CH2:18][CH2:17][O:16][CH2:15][CH2:14]3)[NH:9][C:7]2=[O:8])=[CH:4][CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 27370122-MorpholinobenzonitrileHCID 14839220HCID 14839220, 화합물

생성물 1

HCID 23156849HCID 23156849, 화합물수율 87%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

반응 조건

온도
-78 °C

실험 절차

5.39 ml (9.69 mmol) of a 1.8 M lithium diisopropylamide THF solution was diluted with 10 ml of THF. Thereafter, 5 ml of a THF solution containing 383 mg (1.94 mmol) of the 5-chloro-2,N,N-trimethylbenzamide prepared in Step A of Example 80 was added dropwise to the diluted solution at −78° C. Thereafter, 5 ml of a THF solution containing 438 mg (2.33 mmol) of 2-(4-morpholino)benzonitrile was further added to the above mixture, and the obtained mixture was then stirred at −78° C. for 30 minutes. Thereafter, a saturated ammonium chloride aqueous solution was added to the reaction solution, and the mixture was then extracted with ethyl acetate. The extract was washed with a saturated saline solution, and was then dried over anhydrous sodium sulfate. The resultant was concentrated under reduced pressure. The obtained yellow oily product was crystallized from hexane/ethyl acetate (3:1), so as to obtain 575 mg (87%) of 7-chloro-3-(2-morpholin-4-ylphenyl)-2H-isoquinolin-1-one in the form of a colorless crystal.

후처리

  1. additionwas added dropwise to the diluted solution at −78° C
  2. additionwas further added to the above mixture
  3. extractionthe mixture was then extracted with ethyl acetate
  4. washThe extract was washed with a saturated saline solution
  5. dry with materialwas then dried over anhydrous sodium sulfate
  6. concentrationThe resultant was concentrated under reduced pressure
  7. customThe obtained yellow oily product was crystallized from hexane/ethyl acetate (3:1)

출처 및 근거

ORD 기록
ord-d5f17dbf9bc44c77a7ba34612d1e4c5f
출처 데이터셋
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08143274B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트