Morpholine → HCID 18356993、化合物

HRID 427288ノート

反応式

HRID 427288 の反応式
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

参加物

4

反応物 2

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

生成物 1

HCID 18356993HCID 18356993、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
80 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-7d4636cf4b354785b9610c1928f972ff
出典データセット
uspto-grants-2001_11
特許番号
US06313116B1

反応ノート

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