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Benzyl Alcohol → Phenylmethyl [3-[(3,4-dichlorophenyl)methyl]-2-(1-methylethyl)-3,4,5,6,7,8-hexahydrocyclohepta[d]imidazol-4-yl]acetate

HRID 1946477
ノート
印刷プレビュー

反応式

HRID 1946477 の反応式
N.[Cl:2][C:3]1[CH:4]=[C:5]([CH2:10][N:11]2[C:15]3[CH:16]([CH2:21][C:22]([OH:24])=[O:23])[CH2:17][CH2:18][CH2:19][CH2:20][C:14]=3[N:13]=[C:12]2[CH:25]([CH3:27])[CH3:26])[CH:6]=[CH:7][C:8]=1[Cl:9].[CH2:28](O)[C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1.Cl.CN(C)CCCN=C=NCC>ClCCl.CN(C)C1C=CN=CC=1>[Cl:2][C:3]1[CH:4]=[C:5]([CH2:10][N:11]2[C:15]3[CH:16]([CH2:21][C:22]([O:24][CH2:28][C:29]4[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=4)=[O:23])[CH2:17][CH2:18][CH2:19][CH2:20][C:14]=3[N:13]=[C:12]2[CH:25]([CH3:27])[CH3:26])[CH:6]=[CH:7][C:8]=1[Cl:9]
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

6

反応物 3

HCID 244Benzyl AlcoholHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 67435460[3-[(3,4-Dichlorophenyl)methyl]-2-(1-methylethyl)-3,4,5,6,7,8-hexahydrocyclohepta[d]imidazol-4-yl]acetic acid ammonia salt

生成物 1

HCID 58460204Phenylmethyl [3-[(3,4-dichlorophenyl)methyl]-2-(1-methylethyl)-3,4,5,6,7,8-hexahydrocyclohepta[d]imidazol-4-yl]acetate

試薬・触媒・溶媒 2

HCID 14284
4-(Dimethylamino)pyridine
触媒
HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

To a stirred suspension of Example 3 (180 mg) in dichloromethane (5 mL) at 0° C. was added benzyl alcohol (0.095 mL), 4-dimethylamino pyridine (10 mg) and N′-(3-dimethylaminopropyl)-N-ethylcarbodiimide hydrochloride (100 mg) sequentially. The reaction was stirred at 0° C. under an atmosphere for 1.5 hr. The reaction was allowed to achieve ambient temperature and stirred for a further 18 hr. The reaction mixture was partitioned between dichloromethane (10 mL) and water (10 mL). The aqueous phase was back extracted with dichloromethane (10 mL). The combined organics were dried (hydrophobic frit) and concentrated in vacuo to give 274 mg of product. The sample was purified on silica using 0-100% ethyl acetate-cyclohexane. The appropriate fractions were combined and evaporated in vacuo to give the title compound (159 mg). LC/MS MH+ 485, 487, Rt 2.28 min (5 minute run).

後処理

  1. customto achieve ambient temperature
  2. stirringstirred for a further 18 hr
  3. customThe reaction mixture was partitioned between dichloromethane (10 mL) and water (10 mL)
  4. extractionThe aqueous phase was back extracted with dichloromethane (10 mL)
  5. customThe combined organics were dried (hydrophobic frit)
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-320cb40bd3e14c198b1bb0a57a0299bc
出典データセット
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08399444B2

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