Ammonia → 8-Carbamyl-5-(3-(7-chloroquinolin-2-ylmethylthio)phenyl)-4,6-dithiaoctanoic acid

HRID 22593

反応式

HRID 22593 の反応式
[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[CH:7][C:8]([CH2:12][S:13][C:14]3[CH:15]=[C:16]([CH:20]([S:27][CH2:28][CH2:29][C:30]([OH:32])=O)[S:21][CH2:22][CH2:23][C:24]([OH:26])=[O:25])[CH:17]=[CH:18][CH:19]=3)=[N:9]2)=[CH:4][CH:3]=1.[I-].ClC1C=CC=C[N+:36]=1C.C(N(CC)CC)C.N>ClCCl.C(#N)C.CCOCC>[C:30]([CH2:29][CH2:28][S:27][CH:20]([C:16]1[CH:17]=[CH:18][CH:19]=[C:14]([S:13][CH2:12][C:8]2[CH:7]=[CH:6][C:5]3[C:10](=[CH:11][C:2]([Cl:1])=[CH:3][CH:4]=3)[N:9]=2)[CH:15]=1)[S:21][CH2:22][CH2:23][C:24]([OH:26])=[O:25])(=[O:32])[NH2:36]

参加物

8

反応物 4

HCID 222AmmoniaHCID 8471TriethylamineHCID 1670692-Chloro-1-methylpyridinium iodideHCID 104139205-(3-(7-Chloroquinolin-2-ylmethylthio)phenyl)-4,6-dithianonanedioic acid

生成物 1

HCID 199305208-Carbamyl-5-(3-(7-chloroquinolin-2-ylmethylthio)phenyl)-4,6-dithiaoctanoic acid

試薬・触媒・溶媒 3

HCID 3283Diethyl Ether溶媒HCID 6342Acetonitrile溶媒HCID 6344Dichloromethane溶媒

実験手順

To 500 mg of diacid (Example 20, Step 4) in dichloromethane (39 mL) and acetonitrile (9.9 mL) at 0° C. was added 2-chloro-1-methylpyridinium iodide (315 mg). After 15 min triethylamine (170 μL) and 10 mL of a saturated solution of ammonia in ether were added. The solution was stirred 1 hr at room temperature then it was washed with acidified 25% ammonium acetate, extracted with ethyl acetate, dried over sodium sulfate, filtered and evaporated to dryness. Purification by chromatography afforded the title compound.

後処理

  1. washit was washed
  2. extractionextracted with ethyl acetate
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. customevaporated to dryness
  6. customPurification by chromatography

出典と根拠

ORDレコード
ord-32fdaef34b434ee89b0bff3ed1e90296
出典データセット
uspto-grants-1995_06
特許番号
US05428171

関連ノート

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