Carbon Dioxide → HCID 22459178、化合物

HRID 2184989ノート

反応式

HRID 2184989 の反応式
[CH3:1][O:2][C:3]1[C:16]2[O:15][C:14]3[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=3)[CH2:8][C:7]=2[CH:6]=[CH:5][CH:4]=1.C([N-]C(C)C)(C)C.[Li+].C(=O)=O.COC1C2OC3C(=CC=CC=3)C(C(O)=O)C=2C=CC=1.C(Cl)(=O)[C:48]([Cl:50])=[O:49]>O1CCCC1.C1(C)C=CC=CC=1.CN(C=O)C>[CH3:1][O:2][C:3]1[C:16]2[O:15][C:14]3[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=3)[CH:8]([C:48]([Cl:50])=[O:49])[C:7]=2[CH:6]=[CH:5][CH:4]=1

参加物

8

反応物 5

HCID 280Carbon DioxideHCID 65578Oxalyl chlorideHCID 2724682Lithium diisopropylamideHCID 125543394-Methoxy-9H-xantheneHCID 22459180HCID 22459180、化合物

生成物 1

HCID 22459178HCID 22459178、化合物

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 21735183Dimethylformamide toluene溶媒

実験手順

(RS)-4-Methoxy-9H-xanthene-9-carbonyl chloride was prepared according to general methods described in WO 9706178. 4-Methoxy-xanthene [J.Med.Chem., 32(10), 2357(1989)] was deprotonated with lithium diisopropylamide in tetrahydrofuran followed by treatment with carbon dioxide. The resulting (RS)-4-methoxy-9H-xanthene-9-carboxylic acid (white solid and MS: m/e=256.0 (M+)) was chlorinated with oxalyl chloride in toluene/DMF and yielded after evaporation of the reagent and solvents, the crude acid chloride, which was directly used without further purification.

後処理

  1. customyielded
  2. customafter evaporation of the reagent and solvents
  3. customthe crude acid chloride, which was directly used without further purification

出典と根拠

ORDレコード
ord-cf85ecd894d449fa84316210d753f08b
出典データセット
uspto-grants-2002_06
特許番号
US06399641B1

反応ノート

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