ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Aluminium lithium hydride → HCID 86722363、化合物

HRID 718775
ノート
印刷プレビュー

反応式

HRID 718775 の反応式
[H-].[H-].[H-].[H-].[Li+].[Al+3].[CH2:7]([O:14][C@@:15]1([C:42]([F:45])([F:44])[F:43])[CH2:39][C@H:19]2[CH2:20][CH2:21][CH2:22][C:23]3[C:24](=[CH:25][C:26]4[CH:27]=[N:28][N:29]([C:32]5[CH:37]=[CH:36][C:35]([F:38])=[CH:34][CH:33]=5)[C:30]=4[CH:31]=3)[C@:18]2([C:40]#[N:41])[CH2:17][CH2:16]1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1>CCOCC.C1COCC1>[CH2:7]([O:14][C@@:15]1([C:42]([F:44])([F:45])[F:43])[CH2:39][C@H:19]2[CH2:20][CH2:21][CH2:22][C:23]3[C:24](=[CH:25][C:26]4[CH:27]=[N:28][N:29]([C:32]5[CH:33]=[CH:34][C:35]([F:38])=[CH:36][CH:37]=5)[C:30]=4[CH:31]=3)[C@:18]2([CH2:40][NH2:41])[CH2:17][CH2:16]1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 21226445Aluminium lithium hydrideHCID 86722361HCID 86722361、化合物

生成物 1

HCID 86722363HCID 86722363、化合物

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
0 °C

実験手順

A suspension of LAH (38.0 mg, 1.00 mmol) in ether (1 mL) was stirred under nitrogen and cooled to 0° C. A solution of (3R,4aR,12bS)-3-(benzyloxy)-9-(4-fluorophenyl)-3-(trifluoromethyl)-1,2,3,4,4a,5,6,7,9,12b-decahydrobenzo[6,7]cyclohepta[1,2-f]indazole-12b-carbonitrile (33, R1=4-Fluorophenyl, R3=Trifluoromethyl, Rx=Benzyl) (89 mg, 0.167 mmol) in THF (3 mL) was added maintaining reaction temperature under 5° C. and the mixture was allowed to stir at rt for about 54 h. The reaction was diluted with THF (2 mL) and quenched by addition of water (40 μL), then 2N NaOH (40 μL) and then water (80 μL). The reaction was stirred overnight at rt. The mixture was dried with Na2SO4 and filtered through Celite®, rinsing with THF (5 mL) and EtOAc (10 mL). The combined organics were concentrated under reduced pressure to yield crude ((3R,4aR,12bS)-3-(benzyloxy)-9-(4-fluorophenyl)-3-(trifluoromethyl)-1,2,3,4,4a,5,6,7,9,12b-decahydrobenzo[6,7]cyclohepta[1,2-f]indazol-12b-yl)methanamine (34, R1=4-Fluorophenyl, R3=Trifluoromethyl, Rx=Benzyl). LC/MS, method 3, Rt=2.41 min, MS m/z 538 (M+H)+. The residue was used in step #3 without further purification.

後処理

  1. temperaturemaintaining
  2. customreaction temperature under 5° C.
  3. stirringto stir at rt for about 54 h
  4. customquenched by addition of water (40 μL)
  5. stirringThe reaction was stirred overnight at rt
  6. dry with materialThe mixture was dried with Na2SO4
  7. filtrationfiltered through Celite®
  8. washrinsing with THF (5 mL) and EtOAc (10 mL)
  9. concentrationThe combined organics were concentrated under reduced pressure

出典と根拠

ORDレコード
ord-39c2f07b60744fb89e0a74514d1efe3d
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09193744B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート