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

Ammonia → HCID 23324593、化合物

HRID 1380894
ノート
印刷プレビュー

反応式

HRID 1380894 の反応式
[CH3:1][O:2][C:3]1[C:34]([O:35][CH3:36])=[CH:33][C:6]2[C:7](=[O:32])[C:8](=[O:31])[N:9]([CH2:12][CH2:13][CH2:14][N:15]([CH3:30])[CH:16]3[CH2:25][CH2:24][C:23]4[C:18](=[CH:19][C:20]([O:28][CH3:29])=[C:21]([O:26][CH3:27])[CH:22]=4)[CH2:17]3)[CH2:10][CH2:11][C:5]=2[CH:4]=1.[BH4-].[Na+].Cl.N>CO.O>[OH:32][CH:7]1[C:6]2[CH:33]=[C:34]([O:35][CH3:36])[C:3]([O:2][CH3:1])=[CH:4][C:5]=2[CH2:11][CH2:10][N:9]([CH2:12][CH2:13][CH2:14][N:15]([CH3:30])[CH:16]2[CH2:25][CH2:24][C:23]3[C:18](=[CH:19][C:20]([O:28][CH3:29])=[C:21]([O:26][CH3:27])[CH:22]=3)[CH2:17]2)[C:8]1=[O:31]
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 4

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 4311764Sodium borohydrideHCID 23324574HCID 23324574、化合物

生成物 1

HCID 23324593HCID 23324593、化合物

試薬・触媒・溶媒 1

HCID 22242641Methanol--water (1/1)溶媒

実験手順

Here, 1-[7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-1,2-dion-3-yl]-3-[N-methyl-N-(6,7-dimethoxy-1,2,3,4-tetrahydronaphth-2-yl)-amino]-propane (0.70 g 0.0014 mol) is dissolved in a mixture of methanol/water=(95:5, 21 ml) then sodium borohydride (0.060 g, 0.0016 mol) is added and the mixture is stirred for 20 minutes at ambient temperature. It is then acidified with hydrochloric acid (2 mol/l), made alkaline with methanolic ammonia and extracted with methylene chloride, dried over magnesium sulphate, concentrated by evaporation and the residue is purified over a column [alumina N (50 g), activity II, eluant: methylene chloride and then with increasing amounts of ethanol (up to 3%)]. The residue is dissolved in acetone and mixed with ethereal hydrochloric acid. The precipitate obtained is suction filtered, washed with ether and dried. Yield: 0.18 g. Mp: 141°-143° C.

後処理

  1. extractionextracted with methylene chloride
  2. dry with materialdried over magnesium sulphate
  3. concentrationconcentrated by evaporation
  4. customthe residue is purified over a column [alumina N (50 g), activity II, eluant
  5. dissolutionThe residue is dissolved in acetone
  6. additionmixed with ethereal hydrochloric acid
  7. customThe precipitate obtained
  8. washwashed with ether
  9. customdried

出典と根拠

ORDレコード
ord-3f9b64d63be8490a9140f9cf1c4f28db
出典データセット
uspto-grants-1986_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04584293

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート