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

1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride → Bavisant dihydrochloride anhydrous

HRID 1367617
ノート
印刷プレビュー

反応式

HRID 1367617 の反応式
[ClH:1].[N:2]1([CH2:8][C:9]2[CH:17]=[CH:16][C:12]([C:13]([OH:15])=O)=[CH:11][CH:10]=2)[CH2:7][CH2:6][O:5][CH2:4][CH2:3]1.O.ON1C2C=CC=CC=2N=N1.[CH:29]1([N:32]2[CH2:37][CH2:36][NH:35][CH2:34][CH2:33]2)[CH2:31][CH2:30]1.Cl.CN(C)CCCN=C=NCC>C(#N)C.C1(C)C=CC=CC=1>[ClH:1].[ClH:1].[CH:29]1([N:32]2[CH2:37][CH2:36][N:35]([C:13]([C:12]3[CH:11]=[CH:10][C:9]([CH2:8][N:2]4[CH2:3][CH2:4][O:5][CH2:6][CH2:7]4)=[CH:17][CH:16]=3)=[O:15])[CH2:34][CH2:33]2)[CH2:31][CH2:30]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

7

反応物 4

HCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27292554-(Morpholin-4-ylmethyl)benzoic acid hydrochlorideHCID 27960291-Hydroxybenzotriazole hydrateHCID 47420041-Cyclopropylpiperazine

生成物 1

HCID 66712477Bavisant dihydrochloride anhydrous

試薬・触媒・溶媒 2

HCID 1140
Toluene
溶媒
2 回
HCID 6342Acetonitrile溶媒2 回

反応条件

温度
22.5 °C

実験手順

A 100-L glass-lined reactor was charged with toluene (45.00 kg) and stirred at ˜20-25° C. To the stirring toluene was added 4-(4-morpholinylmethyl)benzoic acid hydrochloride (6.50 kg, 93.5%, 24.04 mol), 1-hydroxybenzotriazole monohydrate (2.32 kg, 15.13 mol), 1-cyclopropylpiperazine (3.50 kg, 27.07 mol) and acetonitrile (9.00 kg). The resulting off-white slurry was stirred under N2 at ˜20-25° C. for 40 minutes. N-(3-Dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (3.50 kg, 27.07 mol) was added, followed by an acetonitrile (1.20 kg) rinse. After the addition, the reaction mixture was stirred at ˜20-25° C. overnight. Water (32.50 kg) and aqueous saturated sodium carbonate (19.50 L) were then added to the stirring suspension. The suspension was stirred for an additional 30 minutes. The resulting biphasic solution was allowed to settle. The aqueous phase was discarded and the organic phase was washed with a 50% brine solution [water (19.50 L)/brine (19.50 L)]. To the stirred organic phase was then added anhydrous sodium sulfate (2.86 kg) and the resulting mixture was stirred at ˜20-25° C. for 1.5 hours. The solid sodium sulfate was filtered off and the filter cake was washed with acetonitrile (15.30 kg). The filtrate was transferred to a clean 100-L glass-lined reactor and stirred at ˜20-25° C. Water (0.47 kg) and 5/6N HCl in 2-propanol were added to precipitate the title compound as the corresponding bis-hydrochloride salt as a solid. The solid was filtered, washed with acetonitrile (10.2 kg) and dried (60 Torr, ˜40-45° C.) to a constant weight to yield the title compound as a white solid.

後処理

  1. stirringThe resulting off-white slurry was stirred under N2 at ˜20-25° C. for 40 minutes
  2. washrinse
  3. additionAfter the addition
  4. stirringthe reaction mixture was stirred at ˜20-25° C. overnight
  5. additionWater (32.50 kg) and aqueous saturated sodium carbonate (19.50 L) were then added to the stirring suspension
  6. stirringThe suspension was stirred for an additional 30 minutes
  7. washthe organic phase was washed with a 50% brine solution [water (19.50 L)/brine (19.50 L)]
  8. stirringadded anhydrous sodium sulfate (2.86 kg) and the resulting mixture was stirred at ˜20-25° C. for 1.5 hours
  9. filtrationThe solid sodium sulfate was filtered off
  10. washthe filter cake was washed with acetonitrile (15.30 kg)
  11. stirringstirred at ˜20-25° C
  12. additionWater (0.47 kg) and 5/6N HCl in 2-propanol were added
  13. customto precipitate the title compound as the corresponding bis-hydrochloride salt as a solid
  14. filtrationThe solid was filtered
  15. washwashed with acetonitrile (10.2 kg)
  16. customdried (60 Torr, ˜40-45° C.) to a constant weight

出典と根拠

ORDレコード
ord-5287753815e44a8bab999a6e612afa92
出典データセット
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07893257B2

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