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Triethylamine → HCID 69075315、化合物

HRID 490271
ノート
印刷プレビュー

反応式

HRID 490271 の反応式
[C:1]([O:5][C:6](=[O:48])[NH:7][C@H:8]([CH2:23][NH:24][C@@H:25]([C:29]1[N:38]([CH2:39][C:40]2[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=2)[C:37](=[O:46])[C:36]2[C:31](=[CH:32][C:33]([Cl:47])=[CH:34][CH:35]=2)[N:30]=1)[CH:26]([CH3:28])[CH3:27])[CH2:9][CH2:10][CH2:11][NH:12][C:13]([O:15][CH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)=[O:14])([CH3:4])([CH3:3])[CH3:2].C(N(CC)CC)C.[C:56]1([CH3:65])[CH:61]=[CH:60][C:59]([C:62](Cl)=[O:63])=[CH:58][CH:57]=1>C1(C)C=CC=CC=1>[C:1]([O:5][C:6](=[O:48])[NH:7][CH:8]([CH2:23][N:24]([CH:25]([C:29]1[N:38]([CH2:39][C:40]2[CH:41]=[CH:42][CH:43]=[CH:44][CH:45]=2)[C:37](=[O:46])[C:36]2[C:31](=[CH:32][C:33]([Cl:47])=[CH:34][CH:35]=2)[N:30]=1)[CH:26]([CH3:28])[CH3:27])[C:62]([C:59]1[CH:60]=[CH:61][C:56]([CH3:65])=[CH:57][CH:58]=1)=[O:63])[CH2:9][CH2:10][CH2:11][NH:12][C:13]([O:15][CH2:16][C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=1)=[O:14])([CH3:3])([CH3:4])[CH3:2]
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

5

反応物 3

HCID 8471TriethylamineHCID 134054-Methylbenzoyl ChlorideHCID 69078749((S)-1-{[(R)-1-(3-Benzyl-7-chloro-4-oxo-3,4-dihydro-quinazolin-2-yl)-2-methyl-propylamino]-methyl}-4-benzyloxycarbonylamino-butyl)-carbamic acid tert-butyl ester

生成物 1

HCID 69075315HCID 69075315、化合物収率 80%

試薬・触媒・溶媒 1

HCID 1140
Toluene
溶媒

反応条件

温度
80 °C

実験手順

To a solution of ((S)-1-{[(R)-1-(3-benzyl-7-chloro-4-oxo-3,4-dihydro-quinazolin-2-yl)-2-methyl-propylamino]-methyl}-4-benzyloxycarbonylamino-butyl)-carbamic acid tert-butyl ester (250 mg, 0.37 mmol) in toluene (4 mL) was added triethylamine (0.10 mL, 0.74 mmol) followed by dropwise addition of p-toluoyl chloride (0.049 mL, 0.37 mmol). The reaction mixture was heated to 80° C. for 18 h, then reflux for 4 h. The reaction mixture was allowed to cool to room temperature, quenched with saturated aqueous NaHCO3 (10 mL) and diluted with CH2Cl2 (10 mL). The extracts were dried over MgSO4, filtered and concentrated under reduced pressure. The residue was purified by silica gel chromatography (3:1 hexanes:ethyl acetate) to provide 235 mg (79%) of the title compound as a pale yellow powder. MS(ES+) m/e 794.2 [M+H]+.

後処理

  1. temperaturereflux for 4 h
  2. temperatureto cool to room temperature
  3. customquenched with saturated aqueous NaHCO3 (10 mL)
  4. additiondiluted with CH2Cl2 (10 mL)
  5. dry with materialThe extracts were dried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customThe residue was purified by silica gel chromatography (3:1 hexanes:ethyl acetate)

出典と根拠

ORDレコード
ord-e9a33926e6ec47dba386599690a92f84
出典データセット
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07528137B2

反応ノート

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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