Trityl chloride → HCID 70604455、化合物

HRID 2163646ノート

反応式

HRID 2163646 の反応式
C(N(CC)CC)C.Cl.[NH2:9][CH:10]1[C:20](=[O:21])[N:12]2[CH:13]([C:18]#[N:19])[C:14]([CH3:17])([CH3:16])[S:15][C@H:11]12.[C:22]1([C:28](Cl)([C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)[C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1>C(Cl)Cl>[C:22]1([C:28]([NH:9][CH:10]2[C:20](=[O:21])[N:12]3[CH:13]([C:18]#[N:19])[C:14]([CH3:16])([CH3:17])[S:15][C@H:11]23)([C:29]2[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=2)[C:35]2[CH:36]=[CH:37][CH:38]=[CH:39][CH:40]=2)[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=1

参加物

5

反応物 3

HCID 6456Trityl chlorideHCID 8471TriethylamineHCID 70604618HCID 70604618、化合物

生成物 1

HCID 70604455HCID 70604455、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Triethylamine (44.5g., 0.44 mole) is added to a slurry of 6-amino-2,2-dimethyl-3-cyanopenam hydrochloride (46.6g., 0.2 mole) in methylene chloride (1500 ml.) at room temperature and the resulting mixture stirred for 20 minutes. Triphenylmethyl chloride (66.9 g., 0.24 mole) is added in one portion to the mixture which is stirred at room temperature for 3.5 hours. The methylene chloride layer is separated and washed with water (5 × 100 ml.). It is then dried (Na3SO4) and concentrated in vacuo to orange-red viscous oil. Methanol (50 ml.) is added and the mixture stirred for a half hour to give a yellow-white solid. The solid is filtered, resuspended in fresh methanol, and the suspension stirred for a half hour. The solid is recovered by filtration and dried in a vacuum oven at room temperature. Yield of crude = 47 gms. M.p. 116-119° C.

後処理

  1. stirringis stirred at room temperature for 3.5 hours
  2. customThe methylene chloride layer is separated
  3. washwashed with water (5 × 100 ml.)
  4. dry with materialIt is then dried (Na3SO4)
  5. concentrationconcentrated in vacuo to orange-red viscous oil
  6. additionMethanol (50 ml.) is added
  7. stirringthe mixture stirred for a half hour
  8. customto give a yellow-white solid
  9. filtrationThe solid is filtered
  10. stirringthe suspension stirred for a half hour
  11. filtrationThe solid is recovered by filtration
  12. customdried in a vacuum oven at room temperature

出典と根拠

ORDレコード
ord-a92c80187538416384978e4bd013bbe5
出典データセット
uspto-grants-1979_01
特許番号
US04136096

反応ノート

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