Morpholine → 1-[5-(3-Cyclobutyl-2,3,4,5-tetrahydro-1H-benzo[d]azepin-7-yloxy)-pyrazin-2-yl]-1-morpholin-4-yl-methanone

HRID 645828ノート

反応式

HRID 645828 の反応式
[NH:1]1[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.[CH:7]1([N:11]2[CH2:17][CH2:16][C:15]3[CH:18]=[C:19]([O:22][C:23]4[N:24]=[CH:25][C:26]([C:29](Cl)=[O:30])=[N:27][CH:28]=4)[CH:20]=[CH:21][C:14]=3[CH2:13][CH2:12]2)[CH2:10][CH2:9][CH2:8]1.CCN(CC1C=CC=CC=1)CC.C=CC1C=CC=CC=1.C=CC1C=CC(C=C)=CC=1>ClCCl>[CH:7]1([N:11]2[CH2:17][CH2:16][C:15]3[CH:18]=[C:19]([O:22][C:23]4[N:24]=[CH:25][C:26]([C:29]([N:1]5[CH2:6][CH2:5][O:4][CH2:3][CH2:2]5)=[O:30])=[N:27][CH:28]=4)[CH:20]=[CH:21][C:14]=3[CH2:13][CH2:12]2)[CH2:8][CH2:9][CH2:10]1

参加物

5

反応物 3

HCID 8083MorpholineHCID 16212021N-benzyl-N-ethylethanamine;1,4-bis(ethenyl)benzene;styreneHCID 866032205-(3-Cyclobutyl-2,3,4,5-tetrahydro-1H-benzo[d]azepin-7-yloxy)-pyrazine-2-carbonyl chloride

生成物 1

HCID 104091851-[5-(3-Cyclobutyl-2,3,4,5-tetrahydro-1H-benzo[d]azepin-7-yloxy)-pyrazin-2-yl]-1-morpholin-4-yl-methanone

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Morpholine (0.17 ml, 2.0 mmol) was added to a stirred solution of the product of step 1 (394 mg, 1 mmol) and diethylaminomethyl polystyrene (1.88 g, 3.2 mmol/g, 6 mmol) in dichloromethane (10 ml). The resulting mixture was allowed to stir at room temperature for 24 hours and the filtered. The filtrate was concentrated in vacuo and the resulting crude residue was purified column chromatography eluting with a mixture of 0.880 ammonia:ethanol:dichloromethane (1:9:90) to afford the title compound (E123). MS (ES+) m/e 409 [M+H]+.

後処理

  1. concentrationThe filtrate was concentrated in vacuo
  2. customthe resulting crude residue was purified column chromatography
  3. washeluting with a mixture of 0.880 ammonia:ethanol:dichloromethane (1:9:90)

出典と根拠

ORDレコード
ord-1b68f372fa994d7385ea9eb1a8f9aa65
出典データセット
uspto-grants-2010_04
特許番号
US07704994B2

反応ノート

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