Hydrochloric Acid → 2-[(9,10-Methanoanthracen-9(10H)-yl)methyl]-4-methylmorpholine

HRID 442520ノート

反応式

HRID 442520 の反応式
[NH:1]1[CH2:6][CH2:5][O:4][CH:3]([CH2:7][C:8]23[CH2:22][CH:15]([C:16]4[CH:17]=[CH:18][CH:19]=[CH:20][C:21]=42)[C:14]2[C:9]3=[CH:10][CH:11]=[CH:12][CH:13]=2)[CH2:2]1.[CH2:23]=O.Cl>C(O)=O>[CH3:23][N:1]1[CH2:6][CH2:5][O:4][CH:3]([CH2:7][C:8]23[CH2:22][CH:15]([C:16]4[CH:17]=[CH:18][CH:19]=[CH:20][C:21]=42)[C:14]2[C:9]3=[CH:10][CH:11]=[CH:12][CH:13]=2)[CH2:2]1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 214150272-[(9,10-Methanoanthracen-9(10H)-yl)methyl]morpholine

生成物 1

HCID 214150012-[(9,10-Methanoanthracen-9(10H)-yl)methyl]-4-methylmorpholine

試薬・触媒・溶媒 1

HCID 284Formic Acid溶媒

反応条件

温度
80 °C

実験手順

A mixture of 9-(2-morpholinylmethyl)-9,10-dihydro-9,10-methanoanthracene (200 mg), formic acid (600 mg) and 37% formalin (0.25 ml) was stirred at 80° C for 2 hours. 4N Hydrochloric acid was added to the cooled reaction mixture, and the reaction mixture was evaporated to dryness. The residue was diluted with water, basified with aqueous ammonia and extracted with ethyl acetate. The ethyl acetate layer was washed with water, dried over anhydrous sodium sulfate and evaporated to dryness to give 9-(4-methyl-2-morpholinylmethyl)-9,10-dihydro-9,10-methanoanthracene, M.P. 136° - 137° C.

後処理

  1. customthe reaction mixture was evaporated to dryness
  2. additionThe residue was diluted with water
  3. extractionextracted with ethyl acetate
  4. washThe ethyl acetate layer was washed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. customevaporated to dryness

出典と根拠

ORDレコード
ord-ff20da63c50b49caac87494fae9fd86e
出典データセット
uspto-grants-1977_08
特許番号
US04045560

反応ノート

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