Trifluoroacetic acid methylene chloride → HCID 68564037、化合物

HRID 970376ノート

反応式

HRID 970376 の反応式
C(OC([N:8]1[CH2:13][CH2:12][C:11]([NH:18][CH2:19][C:20]2[CH:21]=[CH:22][C:23]3[S:28][CH2:27][C:26](=[O:29])[NH:25][C:24]=3[CH:30]=2)([C:14]([F:17])([F:16])[F:15])[CH2:10][CH2:9]1)=O)(C)(C)C.C(O)(C(F)(F)F)=O.C(Cl)Cl>>[F:16][C:14]([F:15])([F:17])[C:11]1([NH:18][CH2:19][C:20]2[CH:21]=[CH:22][C:23]3[S:28][CH2:27][C:26](=[O:29])[NH:25][C:24]=3[CH:30]=2)[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]1

参加物

3

反応物 2

HCID 21863450Trifluoroacetic acid methylene chlorideHCID 68565409HCID 68565409、化合物

生成物 1

HCID 68564037HCID 68564037、化合物

実験手順

A solution of 6-[{1-(tert-butoxycarbonyl)-4-(trifluoromethyl)piperidin-4-ylamino}methyl]-4H-benzo[1,4]thiazin-3-one (3f) in 1:1 TFA/CH2Cl2 is stirred at room temperature until the starting material is consumed, then is concentrated to dryness in vacuo. The residue is partitioned between dilute NaOH and CH2Cl2, and the layers are separated. The aqueous layer is extracted with CH2Cl2, and the combined organic extracts are dried (Na2SO4) and concentrated in vacuo to afford the title compound.

後処理

  1. customis consumed
  2. concentrationis concentrated to dryness in vacuo
  3. customThe residue is partitioned between dilute NaOH and CH2Cl2
  4. customthe layers are separated
  5. extractionThe aqueous layer is extracted with CH2Cl2
  6. dry with materialthe combined organic extracts are dried (Na2SO4)
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-2b8063bc6a994faea6b124db82654275
出典データセット
uspto-grants-2007_12
特許番号
US07312212B2

反応ノート

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