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Hydrochloric Acid → [2-(3-cyclopropyl-2,4-dioxo-3,4-dihydro-2H-quinazolin-1-ylmethyl)-1-(3-methyl-butyl)-1H-benzoimidazol-5-ylmethyl]-carbamic acid tert-butyl ester

HRID 896346
ノート
印刷プレビュー

反応式

HRID 896346 の反応式
[CH:1]1([N:4]2[C:13](=[O:14])[C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[NH:6][C:5]2=[O:15])[CH2:3][CH2:2]1.CC(N=P(N1CCCC1)(N1CCCC1)N1CCCC1)(C)C.[C:37]([O:41][C:42](=[O:61])[NH:43][CH2:44][C:45]1[CH:60]=[CH:59][C:48]2[N:49]([CH2:54][CH2:55][CH:56]([CH3:58])[CH3:57])[C:50]([CH2:52]Cl)=[N:51][C:47]=2[CH:46]=1)([CH3:40])([CH3:39])[CH3:38].Cl>CN(C=O)C>[C:37]([O:41][C:42](=[O:61])[NH:43][CH2:44][C:45]1[CH:60]=[CH:59][C:48]2[N:49]([CH2:54][CH2:55][CH:56]([CH3:57])[CH3:58])[C:50]([CH2:52][N:6]3[C:7]4[C:12](=[CH:11][CH:10]=[CH:9][CH:8]=4)[C:13](=[O:14])[N:4]([CH:1]4[CH2:3][CH2:2]4)[C:5]3=[O:15])=[N:51][C:47]=2[CH:46]=1)([CH3:38])([CH3:40])[CH3:39]
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 313Hydrochloric AcidHCID 3856267tert-Butylimino-tri(pyrrolidino)phosphoraneHCID 172214493-cyclopropyl-1H-quinazoline-2,4-dioneHCID 59561810HCID 59561810、化合物

生成物 1

HCID 69718855[2-(3-cyclopropyl-2,4-dioxo-3,4-dihydro-2H-quinazolin-1-ylmethyl)-1-(3-methyl-butyl)-1H-benzoimidazol-5-ylmethyl]-carbamic acid tert-butyl ester収率 80%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of the 3-cyclopropyl-1H-quinazoline-2,4-dione (148 mg, 0.73 mmol) in DMF (10 mL) was added BTPP (684 mg, 2.19 mmol). After stirring for 20 minutes, [2-chloromethyl-1-(3-methyl-butyl)-1H-benzoimidazol-5-ylmethyl]-carbamic acid tert-butyl ester; HCl salt (294 mg, 0.73 mmol) was added and the resulting mixture was stirred at room temperature overnight. The solvent was removed in vacuo and the residue precipitated from water. The title compound was collected by filtration and extensively washed with water and dried in vacuo to yield [2-(3-cyclopropyl-2,4-dioxo-3,4-dihydro-2H-quinazolin-1-ylmethyl)-1-(3-methyl-butyl)-1H-benzoimidazol-5-ylmethyl]-carbamic acid tert-butyl ester as an off-white solid (310 mg, 80%):

後処理

  1. stirringthe resulting mixture was stirred at room temperature overnight
  2. customThe solvent was removed in vacuo
  3. customthe residue precipitated from water
  4. filtrationThe title compound was collected by filtration
  5. washextensively washed with water
  6. customdried in vacuo

出典と根拠

ORDレコード
ord-416c61d600ae4d5dafd6bb752c73ab04
出典データセット
uspto-grants-2005_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06919331B2

反応ノート

読み込み中…

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