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Hydrochloric Acid → (S)-3-(3-(Aminomethyl)-1,2,3,4-tetrahydroisoquinoline-2-carbonyl)-4-(2-(dibutylamino)pyrimidin-4-yl)-N-(naphthalen-2-ylsulfonyl)benzamide

HRID 529040
ノート
印刷プレビュー

反応式

HRID 529040 の反応式
[CH2:1]([N:5]([CH2:37][CH2:38][CH2:39][CH3:40])[C:6]1[N:11]=[C:10]([C:12]2[CH:20]=[CH:19][C:18]([C:21](=[O:36])[NH:22][S:23]([C:26]3[CH:35]=[CH:34][C:33]4[C:28](=[CH:29][CH:30]=[CH:31][CH:32]=4)[CH:27]=3)(=[O:25])=[O:24])=[CH:17][C:13]=2[C:14](O)=[O:15])[CH:9]=[CH:8][N:7]=1)[CH2:2][CH2:3][CH3:4].[N:41]([CH2:44][C@@H:45]1[CH2:54][C:53]2[C:48](=[CH:49][CH:50]=[CH:51][CH:52]=2)[CH2:47][NH:46]1)=[N+]=[N-].C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.[OH-].[Na+].Cl>C1COCC1>[NH2:41][CH2:44][C@@H:45]1[CH2:54][C:53]2[C:48](=[CH:49][CH:50]=[CH:51][CH:52]=2)[CH2:47][N:46]1[C:14]([C:13]1[CH:17]=[C:18]([CH:19]=[CH:20][C:12]=1[C:10]1[CH:9]=[CH:8][N:7]=[C:6]([N:5]([CH2:37][CH2:38][CH2:39][CH3:40])[CH2:1][CH2:2][CH2:3][CH3:4])[N:11]=1)[C:21]([NH:22][S:23]([C:26]1[CH:35]=[CH:34][C:33]2[C:28](=[CH:29][CH:30]=[CH:31][CH:32]=2)[CH:27]=1)(=[O:25])=[O:24])=[O:36])=[O:15]
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

7

反応物 5

HCID 313Hydrochloric AcidHCID 11776TriphenylphosphineHCID 14798Sodium HydroxideHCID 710607202-(2-(Dibutylamino)pyrimidin-4-yl)-5-(naphthalen-2-ylsulfonylcarbamoyl)benzoic acid2 回HCID 86718892(S)-3-(Azidomethyl)-1,2,3,4-tetrahydroisoquinoline2 回

生成物 1

HCID 70690001
(S)-3-(3-(Aminomethyl)-1,2,3,4-tetrahydroisoquinoline-2-carbonyl)-4-(2-(dibutylamino)pyrimidin-4-yl)-N-(naphthalen-2-ylsulfonyl)benzamide
収率 52%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
50 °C

実験手順

Following a procedure analogous to that for the synthesis of Example 303, 2-(2-(dibutylamino)pyrimidin-4-yl)-5-(naphthalen-2-ylsulfonylcarbamoyl)benzoic acid (Intermediate 303E, 25 mg, 0.05 mmol) was reacted with ((S)-3-(azidomethyl)-1,2,3,4-tetrahydroisoquinoline (Intermediate 92A, 11 mg, 0.06 mmol) and provided a crude oil which was dissolved in THF (1.1 mL). PPh3 (10 mg, 0.014 mmol) was added followed by aq. 0.5N NaOH (100 μL). The resulting reaction mixture was stirred at 50° C. for 1.5 h and then neutralized with 1N HCl solution (100 μL). The volatiles were removed in vacuo, and the residue was purified by preparative HPLC to give the title compound (5 mg, 52%). MS(ESI+) m/z 705.2 (M+H)+.

後処理

  1. customprovided a crude oil which
  2. customThe resulting reaction mixture
  3. customThe volatiles were removed in vacuo
  4. customthe residue was purified by preparative HPLC

出典と根拠

ORDレコード
ord-00e16baba92e4c6e94a5955220834a15
出典データセット
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09346795B2

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