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Hydrochloric Acid → HCID 178513797、化合物

HRID 2406779
ノート
印刷プレビュー

反応式

HRID 2406779 の反応式
[F:1][C:2]([F:13])([F:12])[C@@H:3]1[CH2:8][CH2:7][C@H:6]([C:9]([OH:11])=O)[CH2:5][CH2:4]1.C(Cl)(=O)C(Cl)=O.Cl.Cl.[NH:22]1[CH2:26][CH2:25][CH2:24][C@@H:23]1[CH2:27][O:28][C:29]1[C:30]([C:35]([NH2:37])=[O:36])=[N:31][CH:32]=[CH:33][CH:34]=1.C(N(CC)CC)C.Cl>ClCCl.C(OCC)(=O)C.CN(C)C=O>[F:12][C:2]([F:1])([F:13])[C@@H:3]1[CH2:4][CH2:5][C@H:6]([C:9]([N:22]2[CH2:26][CH2:25][CH2:24][C@@H:23]2[CH2:27][O:28][C:29]2[C:30]([C:35]([NH2:37])=[O:36])=[N:31][CH:32]=[CH:33][CH:34]=2)=[O:11])[CH2:7][CH2:8]1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 66960633(R)-3-(pyrrolidin-2-ylmethoxy)picolinamide dihydrochlorideHCID 178525709HCID 178525709、化合物

生成物 1

HCID 178513797HCID 178513797、化合物収率 58.9%

試薬・触媒・溶媒 3

HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane溶媒3 回HCID 8857Ethyl Acetate溶媒

実験手順

To an ice-cold solution of cis-4-(trifluoromethyl)cyclohexanecarboxylic acid (267 mg, 1.36 mmol) in dichloromethane (5 mL), oxalyl chloride (0.18 mL, 2.04 mmol) and several drop of N,N-dimethylformamide were added. After being stirred at room temperature for 1 h, the mixture was concentrated in vacuo to give a waxy solid. The residual solid was dissolved with dichloromethane (3 mL) and added to the mixture of (R)-3-(pyrrolidin-2-ylmethoxy)picolinamide dihydrochloride (200 mg, 0.68 mmol, EXAMPLE 1 Step 3) and triethylamine (0.48 mL, 3.40 mmol) in dichloromethane (5 mL) at 0° C. After being stirred at 0° C. for 2 h, the mixture was dissolved with ethyl acetate and 2 N hydrochloric acid. The aqueous layer was washed with ethyl acetate, and basified with aq. ammonia. The mixture was extracted with ethyl acetate twice, and washed with brine. The combined extracts were dried over sodium sulfate and concentrated in vacuo to give an amber oil. The residual oil was purified by preparative TLC (methanol/dichloromethane 1:10) to afford 160 mg of the title compound as a colorless viscous oil.

後処理

  1. concentrationthe mixture was concentrated in vacuo
  2. customto give a waxy solid
  3. stirringAfter being stirred at 0° C. for 2 h
  4. washThe aqueous layer was washed with ethyl acetate
  5. extractionThe mixture was extracted with ethyl acetate twice
  6. washwashed with brine
  7. dry with materialThe combined extracts were dried over sodium sulfate
  8. concentrationconcentrated in vacuo
  9. customto give an amber oil
  10. customThe residual oil was purified by preparative TLC (methanol/dichloromethane 1:10)

出典と根拠

ORDレコード
ord-05da438b6c39455c914ec2971e83091e
出典データセット
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08809380B2

反応ノート

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