Morpholine → HCID 18356993, 화합물

HRID 427288노트

반응식

HRID 427288 반응식
Br[C:2]1[S:3][C:4]2[C:10]([Br:11])=[CH:9][CH:8]=[C:7]([O:12][CH3:13])[C:5]=2[N:6]=1.[NH:14]1[CH2:19][CH2:18][O:17][CH2:16][CH2:15]1>O1CCCC1>[Br:11][C:10]1[C:4]2[S:3][C:2]([N:14]3[CH2:19][CH2:18][O:17][CH2:16][CH2:15]3)=[N:6][C:5]=2[C:7]([O:12][CH3:13])=[CH:8][CH:9]=1

참가 물질

4

반응물 2

HCID 8083MorpholineHCID 183569942,7-Dibromo-4-methoxybenzo[d]thiazole

생성물 1

HCID 18356993HCID 18356993, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
80 °C

실험 절차

A suspension of 2,7-dibromo-4-methoxybenzothiazole (1.8 g) and morpholine (10 ml) in tetrahydrofuran (10 ml) was heated at 80° C. for 2 hours. The solvent was removed in vacuo and the residue partitioned between ethyl acetate (100 ml) and water (100 ml). The organic layer was dried over magnesium sulphate (3 g), filtered and the filtrate evaporated in vacuo to yield an off white solid. This was purified by recrystallisation from ethyl acetatelhexane to yield the title compound as a white solid (1.2 g). TLC Rf 0.39 (50% ethyl acetate in hexane).

후처리

  1. customThe solvent was removed in vacuo
  2. customthe residue partitioned between ethyl acetate (100 ml) and water (100 ml)
  3. dry with materialThe organic layer was dried over magnesium sulphate (3 g)
  4. filtrationfiltered
  5. customthe filtrate evaporated in vacuo
  6. customto yield an off white solid
  7. customThis was purified by recrystallisation from ethyl acetatelhexane

출처 및 근거

ORD 기록
ord-7d4636cf4b354785b9610c1928f972ff
출처 데이터셋
uspto-grants-2001_11
특허 번호
US06313116B1

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