Hydrochloric Acid → HCID 59483836、化合物

HRID 1808378ノート

反応式

HRID 1808378 の反応式
Cl.[N:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:37][CH2:36][C:11]3([CH2:16][CH2:15][N:14]([C:17]([C:19]4[CH:28]=[C:27]5[C:22]([CH2:23][CH2:24][N:25](C(OC(C)(C)C)=O)[CH2:26]5)=[CH:21][CH:20]=4)=[O:18])[CH2:13][CH2:12]3)[CH2:10][CH2:9]2)=[CH:4][CH:3]=1>CO>[N:2]1[CH:3]=[CH:4][C:5]([N:8]2[CH2:37][CH2:36][C:11]3([CH2:12][CH2:13][N:14]([C:17]([C:19]4[CH:28]=[C:27]5[C:22]([CH2:23][CH2:24][NH:25][CH2:26]5)=[CH:21][CH:20]=4)=[O:18])[CH2:15][CH2:16]3)[CH2:10][CH2:9]2)=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 59483838HCID 59483838、化合物

生成物 1

HCID 59483836HCID 59483836、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

1.25 M hydrogen chloride in methanol (15.5 ml, 19.36 mmol) was added at RT to a solution of tert-butyl 7-(9-(pyridin-4-yl)-3,9-diazaspiro[5.5]undecane-3-carbonyl)-3,4-dihydroisoquinoline-2(1H)-carboxylate (1.9 g, 3.87 mmol) in methanol (4 ml), and the reaction mixture was refluxed for 1.5 h. The solvent was removed in vacuo, the residue was taken up in a small amount of ethanol (3 ml), and diethyl ether (50 ml) was added. The mixture was then cooled for 30 min in an ice bath, and the resulting solid was filtered out, washed with diethyl ether and dried in vacuo. Yield: 1.56 g (94%).

後処理

  1. temperaturethe reaction mixture was refluxed for 1.5 h
  2. customThe solvent was removed in vacuo
  3. additionwas added
  4. temperatureThe mixture was then cooled for 30 min in an ice bath
  5. filtrationthe resulting solid was filtered out
  6. washwashed with diethyl ether
  7. customdried in vacuo

出典と根拠

ORDレコード
ord-16cb9eb322f44de5b83f7353ec04cb6d
出典データセット
uspto-grants-2013_01
特許番号
US08357717B2

反応ノート

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