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Hydrochloric Acid → trans-N-(7-Amino-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl)-2,2,2-trifluoroacetamide

HRID 16179
ノート
印刷プレビュー

反応式

HRID 16179 の反応式
[F:1][C:2]([F:34])([F:33])[C:3]([NH:5][C@H:6]1[C@@H:16]2[N:10]([C:11]3[CH:24]=[C:23]([NH:25]CC4C=CC=CC=4)[CH:22]=[CH:21][C:12]=3[O:13][C:14]3[CH:20]=[CH:19][CH:18]=[CH:17][C:15]=32)[CH2:9][CH2:8][CH2:7]1)=[O:4].Cl.O1CCOCC1>C(O)C.[Pd]>[NH2:25][C:23]1[CH:22]=[CH:21][C:12]2[O:13][C:14]3[CH:20]=[CH:19][CH:18]=[CH:17][C:15]=3[C@@H:16]3[C@H:6]([NH:5][C:3](=[O:4])[C:2]([F:33])([F:34])[F:1])[CH2:7][CH2:8][CH2:9][N:10]3[C:11]=2[CH:24]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 86599889trans-2,2,2-trifluoro-N-[2,3,4,14b-tetrahydro-7-[(phenylmethyl)amino]-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl]acetamide

生成物 1

HCID 86599890trans-N-(7-Amino-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl)-2,2,2-trifluoroacetamide収率 53%

試薬・触媒・溶媒 2

HCID 23938
Palladium
触媒
HCID 702Ethanol溶媒

実験手順

To a solution of trans-2,2,2-trifluoro-N-[2,3,4,14b-tetrahydro-7-[(phenylmethyl)amino]-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl]acetamide (944 mg, 2.0 mmol) in ethanol (16 mL) were added Pd/C 10% (111 mg) and a solution of 4M HCl in dioxane (778 μl, 3.11 mmol). The resulting reaction mixture was hydrogenated at 3 bar for 6 h. The reaction mixture was quenched with sat. NaHCO3 (aq) and diluted with ethanol. After filtration through dicalite and thorough washing with ethyl acetate, the volatiles were removed in vacuo. A part of the crude product was purified with HPLC to afford the title compound (29 mg, 53%). Data (m/z)=378 (M+H)+.

後処理

  1. customThe resulting reaction mixture
  2. customThe reaction mixture was quenched with sat. NaHCO3 (aq)
  3. additiondiluted with ethanol
  4. filtrationAfter filtration through dicalite
  5. washthorough washing with ethyl acetate
  6. customthe volatiles were removed in vacuo
  7. customA part of the crude product was purified with HPLC

出典と根拠

ORDレコード
ord-62780275474946fcb37d7b069485186d
出典データセット
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07737136B2

反応ノート

読み込み中…

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