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Citric Acid → HCID 86607736、化合物

HRID 1752886
ノート
印刷プレビュー

反応式

HRID 1752886 の反応式
C(=O)([O-])[O-].[K+].[K+].Br[C:8]1[CH:9]=[C:10]([CH:20]=[CH:21][C:22]=1[O:23][CH2:24][O:25][CH2:26][CH2:27][O:28][CH3:29])[CH2:11][NH:12][C:13]([NH:15][C:16]([CH3:19])([CH3:18])[CH3:17])=[O:14].[CH3:30][O:31][CH2:32][CH2:33][O:34][CH2:35][O:36][C:37]1[C:44](B2OC(C)(C)C(C)(C)O2)=[CH:43][CH:42]=[CH:41][C:38]=1[CH:39]=[O:40].C(O)(=O)CC(CC(O)=O)(C(O)=O)O>C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.C(OCC)(=O)C>[C:16]([NH:15][C:13]([NH:12][CH2:11][C:10]1[CH:9]=[C:8]([C:44]2[CH:43]=[CH:42][CH:41]=[C:38]([CH:39]=[O:40])[C:37]=2[O:36][CH2:35][O:34][CH2:33][CH2:32][O:31][CH3:30])[C:22]([O:23][CH2:24][O:25][CH2:26][CH2:27][O:28][CH3:29])=[CH:21][CH:20]=1)=[O:14])([CH3:19])([CH3:18])[CH3:17]
参加物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 311Citric AcidHCID 11430Potassium CarbonateHCID 66986052HCID 66986052、化合物HCID 86607704HCID 86607704、化合物

生成物 1

HCID 86607736HCID 86607736、化合物収率 56.4%

試薬・触媒・溶媒 2

HCID 178418397
HCID 178418397、化合物
触媒
HCID 8857Ethyl Acetate溶媒

実験手順

A 2 M solution of potassium carbonate (2.1 mL) was added to a magnetically stirred mixture of 1-[3-bromo-4-(2-methoxyethoxymethoxy)benzyl]-3-tert-butylurea (1.4 g, 4.1 mmol), prepared as in Reference 11, and 2-(2-methoxyethoxymethoxy)-3-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-benzaldehyde (42 mL, 0.1 mM in toluene, 4.2 mmol), prepared as in Reference 15. The mixture was flushed with nitrogen and then tetrakis(triphenylphosphine)palladium(0) (118 mg, 0.1025 mmol) was added. The mixture was refluxed for 7 hours, cooled and then poured into a mixture of ethyl acetate and 5% citric acid. The organic phase was separated and the aqueous phase was extracted twice more with ethyl acetate. The combined organic phase was dried and concentrated by evaporation. Product was purified from the residue by chromatography on silica gel utilizing 100% ethyl acetate to give 1-tert-butyl-3-[3′-formyl-6,2′-bis-(2-methoxyethoxymethoxy)-biphenyl-3-ylmethyl]-urea (1.2 g).

後処理

  1. customThe mixture was flushed with nitrogen
  2. temperatureThe mixture was refluxed for 7 hours
  3. temperaturecooled
  4. customThe organic phase was separated
  5. extractionthe aqueous phase was extracted twice more with ethyl acetate
  6. customThe combined organic phase was dried
  7. concentrationconcentrated by evaporation
  8. customProduct was purified from the residue by chromatography on silica gel utilizing 100% ethyl acetate

出典と根拠

ORDレコード
ord-26586a4f4c25487dac7ecc2167dc309c
出典データセット
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09162986B2

反応ノート

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