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Acetic Acid → HCID 67166102、化合物

HRID 553291
ノート
印刷プレビュー

反応式

HRID 553291 の反応式
[OH-].[Li+].C[O:4][C:5](=[O:29])[CH2:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([CH2:19][N:20]3[CH2:28][C:27]4[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=4)[CH2:21]3)[CH:14]=2)=[CH:9][CH:8]=1.C(O)(=O)C>O.O1CCCC1>[CH2:21]1[C:22]2[C:27](=[CH:26][CH:25]=[CH:24][CH:23]=2)[CH2:28][N:20]1[CH2:19][C:15]1[CH:14]=[C:13]([C:10]2[CH:9]=[CH:8][C:7]([CH2:6][C:5]([OH:29])=[O:4])=[CH:12][CH:11]=2)[CH:18]=[CH:17][CH:16]=1
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 3

HCID 176Acetic AcidHCID 3939Lithium HydroxideHCID 67165602HCID 67165602、化合物

生成物 1

HCID 67166102HCID 67166102、化合物収率 99.7%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Lithium hydroxide (126 mg) in water (5 mL) was added to a solution of [3′-(1,3-dihydro-iso-indol-2-ylmethyl)-biphenyl-4-yl]-acetic acid methyl ester (0.47 g) in tetrahydrofuran (10 mL) and stirred at room temperature for 72 hour. The reaction mixture was acidified with glacial acetic acid and evaporated. The residue was partitioned between ethyl acetate (20 mL) and water (20 mL). The aqueous was separated and extracted with ethyl acetate (2×20 mL). The combined organics were washed with brine (20 mL), dried (sodium sulfate) and evaporated to give a the subtitle compound as a brown oil (450 mg).

後処理

  1. customevaporated
  2. customThe residue was partitioned between ethyl acetate (20 mL) and water (20 mL)
  3. customThe aqueous was separated
  4. extractionextracted with ethyl acetate (2×20 mL)
  5. washThe combined organics were washed with brine (20 mL)
  6. dry with materialdried (sodium sulfate)
  7. customevaporated

出典と根拠

ORDレコード
ord-e2c88c591f7d4036a7a45010542c6dc0
出典データセット
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07951954B2

反応ノート

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